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在标题化合物的分子量中,C31H(H)272,二氢吡啶环和环己烯环分别采用扁平ed-boat构象和包络构象。分子间C-H连接分子...O氢键,形成链状结构。

支持信息

到岸价

结晶信息文件(CIF)https://doi.org/10.107/S1600536806015303/hk2032sup1.cif
包含全局数据块,I

香港特别行政区

结构系数文件(CIF格式)https://doi.org/10.107/S1600536806015303/hk2032Isup2.hkl
包含数据块I

CCDC参考:603120

关键指标

  • 单晶X射线研究
  • T型=173 K
  • 平均值[西格玛](C-C)=0.003º
  • R(右)系数=0.056
  • 水风险系数=0.110
  • 数据与参数之比=13.4

检查CIF/PLATON结果

未发现语法错误
警报级别C PLAT063_警报_3_C晶体对于光束尺寸来说可能太大。。。。。。。0.79毫米PLAT066_警报_1_C预测和报告的传输相同?
0A级警报=一般情况:严重问题0B级警报=潜在的严重问题2C级警报=检查并解释0G级警报=一般警报;检查1警报类型1 CIF结构/语法错误,数据不一致或缺失0警报类型2结构模型可能错误或有缺陷的指示器1警报类型3结构质量可能较低的指示器0警报类型4改进、方法、查询或建议

计算详细信息顶部

数据收集:智能(布鲁克,1998);单元格细化:智能; 数据缩减:圣保罗(布鲁克,1999);用于求解结构的程序:SHELXS97标准(谢尔德里克,1997);用于优化结构的程序:SHELXL97型(谢尔德里克,1997);分子图形:SHELXTL公司(布鲁克,1999);用于准备出版材料的软件:SHELXTL公司.

10-苄基-7,8-二氢-7,7-二甲基-5-苯基-5H(H)-茚并[1,2-b条]喹啉-9,11(6H(H),10H)-二酮顶部
水晶数据 顶部
C31H(H)272F类(000) = 944
M(M)第页= 445.54D类x=1.307毫克
单诊所,P(P)21/n个熔点=480–482 K
大厅符号:-P 2ynK(K)α辐射,λ= 0.71070 Å
= 14.783 (2) Å7710次反射的细胞参数
b条= 9.4408 (12) Åθ= 3.0–25.3°
c= 16.345 (2) ŵ=0.08毫米1
β= 96.878 (3)°T型=173 K
V(V)= 2264.6 (5) Å块,红色
Z轴= 40.79×0.32×0.14毫米
数据收集 顶部
Rigaku Mercury公司
衍射仪
4144个独立反射
辐射源:细焦点密封管3611次反射> 2σ()
石墨单色仪R(右)整数= 0.040
探测器分辨率:7.31像素mm-1θ最大值= 25.4°,θ最小值= 3.3°
ω扫描小时=1717
吸收校正:多扫描
(SADABS;谢尔德里克,1996年)
k个=1111
T型最小值= 0.939,T型最大值= 0.989=1919
21579次测量反射
精炼 顶部
优化于F类2主原子位置定位:结构-变量直接方法
最小二乘矩阵:完整二次原子位置:差分傅里叶映射
R(右)[F类2> 2σ(F类2)] = 0.056氢站点位置:从邻近站点推断
水风险(F类2) = 0.110受约束的氢原子参数
S公司= 1.18 w个= 1/[σ2(F类o(o)2) + (0.0325P(P))2+ 0.9725P(P)]
哪里P(P)= (F类o(o)2+ 2F类c2)/3
4144次反射(Δ/σ)最大值< 0.001
310参数Δρ最大值=0.20埃
0个约束Δρ最小值=0.18埃
特殊细节 顶部

实验.1核磁共振氢谱(二甲基亚砜-d6,δ,下午):7.52–7.61(m,4H,ArH),7.34(d,1H,ArH,J=6.8赫兹),7.18–7.26(米,4H,氩),6.94(吨,1H,氩,J=7.6赫兹),ArH,J=6.8 Hz),6.21(s,1H,ArH),4.91,1H,CH,J=3.8 Hz),2.78–2.87(m,2H,CH2),2.28(秒,2H,CH2),2.16(d,1H,瑞士2,J=17.6 Hz),1.63(d,1H,CH2,J=17.6 Hz),0.93(s,3H,中国),0.91(s,3H,CH).

几何图形.所有e.s.d.(两个l.s.平面之间二面角的e.s.d.除外)使用全协方差矩阵进行估计在估计e.s.d.的距离、角度时单独考虑和扭转角;e.s.d.细胞内参数之间的相关性仅为当它们由晶体对称性定义时使用。近似(各向同性)细胞e.s.d.的处理用于估计涉及l.s.的e.s.d。飞机。

精炼.改进F类2针对所有反射。加权R(右)-因子水风险和贴合度S公司基于F类2,常规R(右)-因素R(右)基于F类,使用F类设置为零消极的F类2。的阈值表达式F类2>σ(F类2)仅用于计算R(右)-因子(gt).并且与选择反射进行细化无关。R(右)-基于的因素F类2从统计上看大约是两倍大作为那些基于F类、和R(右)-基于所有数据的系数将为甚至更大。

分数原子坐标和各向同性或等效各向同性位移参数2) 顶部
xz(z)U型国际标准化组织*/U型等式
O1公司1.07434 (10)0.80923 (16)0.54032 (9)0.0447 (4)
氧气0.79919 (10)0.74458 (14)0.73821 (8)0.0396 (4)
N1型0.79564 (10)0.56606 (16)0.46614 (9)0.0268 (4)
C10.88118 (12)0.62213 (19)0.46130 (11)0.0265 (4)
指挥与控制0.92401 (12)0.7058 (2)0.52096 (12)0.0287 (4)
C3类0.88337 (13)0.75617 (19)0.59465 (12)0.0287 (4)
H3级0.92800.73520.64410.034*
补体第四成份0.79891 (12)0.66795 (19)0.60181 (11)0.0261 (4)
C5级0.75762 (12)0.58513 (19)0.54035 (11)0.0249 (4)
C6级1.01483 (13)0.7402 (2)0.49968 (13)0.0332 (5)
抄送71.02140 (13)0.6719 (2)0.41787 (12)0.0322 (5)
抄送81.09108 (14)0.6730 (2)0.36971 (14)0.0391 (5)
H8型1.14510.72560.38570.047*
C9级1.08106 (14)0.5954 (2)0.29670 (14)0.0410 (5)
H9型1.12800.59670.26180.049*
C10号机组1.00340 (14)0.5168 (2)0.27496 (13)0.0390 (5)
H10型0.99840.46220.22580.047*
C11号机组0.93145 (14)0.5157 (2)0.32393 (12)0.0339 (5)
H11型0.87810.46130.30840.041*
第12项0.94043 (13)0.5955 (2)0.39501 (12)0.0294 (4)
第13页0.76267 (13)0.67117 (19)0.68133 (11)0.0288 (4)
第14项0.68374 (13)0.5779 (2)0.69386 (11)0.0285 (4)
H14A型0.65020.62070.73660.034*
H14B型0.70730.48500.71480.034*
第15项0.61742 (12)0.55395 (19)0.61619 (11)0.0275 (4)
第16号0.67250 (12)0.5017 (2)0.54825 (11)0.0272 (4)
H16A型0.68950.40150.55940.033*
H16B型0.63300.50490.49490.033*
第17页0.56774 (14)0.6921 (2)0.59078 (13)0.0380 (5)
H17A型0.53650.72680.63640.057*
H17B型0.52300.67500.54250.057*
H17C型0.61190.76310.57710.057*
第18页0.54838 (13)0.4415 (2)0.63422 (12)0.0354 (5)
H18A型0.58050.35430.65270.053*
H18B型0.50690.42220.58410.053*
H18C型0.51330.47580.67750.053*
第19号0.74301 (12)0.5104 (2)0.39283 (11)0.0271 (4)
C20个0.72866 (13)0.3666 (2)0.38307 (12)0.0330 (5)
H20(H20)0.75230.30190.42480.040*
C21型0.67891 (14)0.3184 (2)0.31098 (13)0.0387 (5)
H21型0.66750.21980.30400.046*
C22型0.64589 (14)0.4108 (2)0.24959 (12)0.0381 (5)
硫化氢0.61220.37590.20060.046*
C23型0.66172 (13)0.5544 (2)0.25904 (12)0.0370 (5)
H23(H23)0.63980.61850.21640.044*
C24型0.70992 (13)0.6043 (2)0.33137 (11)0.0314 (4)
硫酸0.72020.70310.33870.038*
C25型0.86565 (13)0.9194 (2)0.59340 (12)0.0324 (5)
硫化氢5a0.86500.95230.65080.039*
H25B型0.91710.96700.57120.039*
C26型0.77827 (13)0.96529 (19)0.54351 (12)0.0297 (4)
C27型0.76343 (15)0.9440 (2)0.45905 (12)0.0375 (5)
H27型0.81020.90300.43160.045*
C28型0.68174 (16)0.9813 (2)0.41408 (14)0.0450 (6)
第28页0.67220.96350.35650.054*
C29型0.61387 (15)1.0444 (2)0.45278 (14)0.0435 (5)
H29型0.55751.06930.42210.052*
C30型0.62869 (15)1.0707 (2)0.53576 (14)0.0410 (5)
H30型0.58311.11660.56240.049*
C31号机组0.70966 (15)1.0306 (2)0.58081 (13)0.0370 (5)
第31页0.71861.04800.63850.044*
原子位移参数(2) 顶部
U型11U型22U型33U型12U型13U型23
O1公司0.0331 (8)0.0468 (9)0.0527 (10)0.0118 (7)0.0008 (7)0.0021 (7)
氧气0.0499 (9)0.0392 (8)0.0289 (8)0.0091 (7)0.0015 (7)0.0048 (6)
N1型0.0246 (8)0.0318 (9)0.0238 (8)0.0034 (7)0.0017 (6)0.0015 (6)
C10.0227 (9)0.0249 (9)0.0314 (10)0.0017 (8)0.0013 (8)0.0071 (8)
指挥与控制0.0258 (10)0.0275 (10)0.0321 (11)0.0010 (8)0.0007 (8)0.0051 (8)
C3类0.0286 (10)0.0294 (10)0.0269 (10)0.0036 (8)0.0019 (8)0.0027 (8)
补体第四成份0.0252 (9)0.0247 (9)0.0276 (10)0.0007 (8)0.0001 (8)0.0044 (8)
C5级0.0247 (9)0.0257 (9)0.0237 (9)0.0025 (8)0.0004 (7)0.0038 (7)
C6级0.0298 (11)0.0281 (10)0.0406 (12)0.0008 (9)0.0005 (9)0.0098 (9)
抄送70.0278 (10)0.0306 (10)0.0381 (11)0.0026 (9)0.0035 (8)0.0112 (9)
抄送80.0288 (11)0.0395 (12)0.0499 (14)0.0028 (9)0.0085 (10)0.0146 (10)
C9级0.0326 (11)0.0479 (13)0.0456 (13)0.0143 (10)0.0175 (10)0.0185 (10)
C10号机组0.0381 (12)0.0464 (12)0.0338 (12)0.0131 (10)0.0094 (9)0.0073 (9)
C11号机组0.0296 (10)0.0395 (11)0.0327 (11)0.0052 (9)0.0039 (9)0.0071 (9)
第12项0.0278 (10)0.0297 (10)0.0310 (11)0.0049 (8)0.0045 (8)0.0096 (8)
第13页0.0338 (10)0.0260 (10)0.0253 (10)0.0018 (8)0.0017 (8)0.0011 (8)
第14项0.0315 (10)0.0315 (10)0.0228 (10)0.0009 (8)0.0037 (8)0.0018 (8)
第15项0.0262 (10)0.0301 (10)0.0265 (10)0.0015 (8)0.0044 (8)0.0018 (8)
第16号0.0244 (10)0.0303 (10)0.0266 (10)0.0008 (8)0.0017 (8)0.0009 (8)
第17页0.0350 (11)0.0403 (12)0.0379 (12)0.0079 (10)0.0012 (9)0.0010 (9)
第18页0.0288 (10)0.0433 (12)0.0347 (11)0.0034 (9)0.0058 (9)0.0009 (9)
第19号0.0230 (9)0.0339 (10)0.0248 (10)0.0020 (8)0.0047 (8)0.0032 (8)
C20个0.0354 (11)0.0330 (11)0.0319 (11)0.0021 (9)0.0088 (9)0.0016 (8)
C21型0.0427 (12)0.0369 (12)0.0383 (12)0.0095 (10)0.0125 (10)0.0120 (9)
C22型0.0339 (11)0.0531 (14)0.0276 (11)0.0082 (10)0.0044 (9)0.0119 (10)
C23型0.0332 (11)0.0499 (13)0.0274 (11)0.0006 (10)0.0021 (9)0.0024 (9)
C24型0.0316 (11)0.0333 (11)0.0294 (10)0.0005 (9)0.0036 (8)0.0001 (8)
C25型0.0352 (11)0.0296 (10)0.0322 (11)0.0056 (9)0.0032 (9)0.0027 (8)
C26型0.0377 (11)0.0210 (9)0.0309 (11)0.0043 (8)0.0063 (9)0.0014 (8)
第27页0.0483 (13)0.0327 (11)0.0317 (11)0.0094 (10)0.0060 (10)0.0018 (9)
C28型0.0624 (15)0.0361 (12)0.0338 (12)0.0125 (11)0.0048 (11)0.0012 (9)
C29型0.0432 (13)0.0326 (12)0.0521 (14)0.0069 (10)0.0047 (11)0.0021 (10)
C30型0.0426 (13)0.0316 (11)0.0505 (14)0.0049 (10)0.0127 (11)0.0009 (10)
C31号机组0.0465 (13)0.0316 (11)0.0333 (11)0.0020 (10)0.0066 (10)0.0002 (9)
几何参数(λ,º) 顶部
O1-C6型1.224 (2)C16-H16A型0.9900
氧气-C131.231 (2)C16-H16B型0.9900
N1-C1型1.382 (2)C17-H17A型0.9800
N1-C5型1.408 (2)C17-H17B型0.9800
N1-C19号机组1.447 (2)C17-H17C型0.9800
C1-C2类1.352 (3)C18-H18A型0.9800
C1-C12号机组1.494 (3)C18-H18B型0.9800
C2-C6型1.463 (3)C18-H18C型0.9800
C2-C3型1.487 (3)C19-C20型1.381 (3)
C3-C4型1.517 (3)C19-C24号1.385 (3)
C3-C25型1.562 (3)C20-C21型1.389 (3)
C3至H31C20-H20型0.9500
C4-C5型1.359 (3)C21-C221.374 (3)
C4-C13型1.464 (3)C21-H21型0.9500
C5至C161.503 (3)C22-C23型1.382 (3)
C6至C71.498 (3)C22-H22型0.9500
C7-C8号机组1.369 (3)C23-C24型1.388 (3)
C7-C12号机组1.409 (3)C23-H23型0.9500
C8-C9型1.393 (3)C24-H24型0.9500
C8-H8型0.9500C25-C26型1.506 (3)
C9-C10型1.377 (3)C25-H25A型0.9900
C9-H90.9500C25-H25B型0.9900
C10-C11号机组1.406 (3)C26-C27型1.386 (3)
C10-H10型0.9500C26-C31型1.389 (3)
C11-C121.378 (3)C27-C28型1.382 (3)
C11-H11型0.9500C27小时27分0.9500
C13至C141.495 (3)C28-C29型1.383 (3)
C14-C15号1.525 (2)C28-H28型0.9500
C14-H14A型0.9900C29-C30型1.370 (3)
C14-H14B型0.9900C29-H29型0.9500
C15至C181.525 (3)C30-C31型1.381 (3)
C15-C17号1.530 (3)C30-H30型0.9500
C15至C161.535 (3)C31-H310.9500
C1-N1-C5117.56 (15)C15-C16-H16A型108.6
C1-N1-C19119.78 (15)C5-C16-H16B型108.6
C5-N1-C19121.95 (14)C15-C16-H16B型108.6
C2-C1-N1型122.36 (17)H16A-C16-H16B型107.6
C2-C1-C12型110.91 (16)C15-C17-H17A109.5
N1-C1-C12126.65 (16)C15-C17-H17B109.5
C1-C2-C6型108.80 (17)H17A-C17-H17B型109.5
C1-C2-C3124.85 (17)C15-C17-H17C型109.5
C6-C2-C3126.33 (17)H17A-C17-H17C型109.5
C2-C3-C4型107.63 (15)H17B-C17-H17C型109.5
C2-C3-C25型112.85 (16)C15-C18-H18A型109.5
C4-C3-C25型113.84 (16)C15-C18-H18B型109.5
C2-C3-H3型107.4H18A-C18-H18B109.5
C4-C3-H3型107.4C15-C18-H18C型109.5
C25-C3-H3型107.4H18A-C18-H18C109.5
C5-C4-C13型119.24 (17)H18B-C18-H18C型109.5
C5-C4-C3124.05 (17)C20-C19-C24型120.66 (18)
C13-C4-C3型116.69 (16)C20-C19-N1型120.85 (17)
C4-C5-N1型121.34 (16)C24-C19-N1型118.45 (17)
C4-C5-C16型123.00 (17)C19-C20-C21号118.61 (19)
N1-C5-C16115.57 (15)C19-C20-H20型120.7
O1-C6-C2型127.5 (2)C21-C20-H20型120.7
O1-C6-C7型126.45 (19)C22-C21-C20型121.13 (19)
C2-C6-C7型106.00 (16)C22-C21-H21型119.4
C8-C7-C12型121.7 (2)C20-C21-H21型119.4
C8-C7-C6130.04 (19)C21-C22-C23型120.07 (19)
C12-C7-C6108.27 (17)C21-C22-H22120
C7-C8-C9118.6 (2)C23-C22-H22型120
C7-C8-H8型120.7C22-C23-C24型119.42 (19)
C9-C8-H8120.7C22-C23-H23型120.3
C10-C9-C8号机组120.28 (19)C24-C23-H23型120.3
C10-C9-H9型119.9C19-C24-C23型120.09 (19)
C8-C9-H9型119.9C19-C24-H24型120
C9-C10-C11121.4 (2)C23-C24-H24型120
C9-C10-H10119.3C26-C25-C3型114.99 (15)
C11-C10-H10型119.3C26-C25-H25A型108.5
C12-C11-C10118.2 (2)C3-C25-H25A型108.5
C12-C11-H11型120.9C26-C25-H25B型108.5
C10-C11-H11号机组120.9C3-C25-H25B型108.5
C11-C12-C7型119.78 (18)H25A-C25-H25B型107.5
C11-C12-C1134.27 (18)C27-C26-C31型117.69 (19)
C7-C12-C1105.93 (16)C27-C26-C25型121.36 (18)
O2-C13-C4120.53 (17)C31-C26-C25型120.94 (18)
氧气-C13-C14120.46 (17)C28-C27-C26型121.1 (2)
C4-C13-C14型118.94 (16)C28-C27-H27型119.4
C13-C14-C15型114.06 (15)C26-C27-H27型119.4
C13-C14-H14A型108.7C27-C28-C29型120.1 (2)
C15-C14-H14A108.7C27-C28-H28型119.9
C13-C14-H14B108.7C29-C28-H28型119.9
C15-C14-H14B108.7C30-C29-C28型119.5 (2)
H14A-C14-H14B107.6C30-C29-H29型120.3
C14-C15-C18型108.71 (15)C28-C29-H29型120.3
C14-C15-C17型109.84 (16)C29-C30-C31120.3 (2)
C18-C15-C17型109.59 (16)C29-C30-H30型119.9
C14-C15-C16107.82 (15)C31-C30-H30119.9
C18-C15-C16型109.95 (15)C30-C31-C26121.3 (2)
C17-C15-C16型110.90 (16)C30-C31-H31119.3
C5-C16-C15114.56 (15)C26-C31-H31型119.3
C5-C16-H16A108.6
C5-N1-C1-C27.2 (2)C2-C1-C12-C11177.2 (2)
C19-N1-C1-C2型163.38 (17)N1-C12-C110.2 (3)
C5-N1-C1-C12169.48 (16)C2-C1-C12-C7型1.4 (2)
C19-N1-C1-C1220.0 (3)N1-C12-C7型178.38 (16)
N1-C1-C2-C6型176.65 (16)C5-C4-C13-O2179.50 (17)
C12-C1-C2-C60.5 (2)C3-C4-C13-O21.2 (3)
N1-C1-C2-C34.7 (3)C5-C4-C13-C142.8 (3)
C12-C1-C2-C3178.16 (16)C3-C4-C13-C14175.49 (16)
C1-C2-C3-C4型14.6 (2)O2-C13-C14-C15型150.56 (17)
C6-C2-C3-C4型166.99 (17)C4-C13-C14-C1532.7 (2)
C1-C2-C3-C25111.8 (2)C13-C14-C15-C18172.02 (16)
C6-C2-C3-C2566.6 (2)C13-C14-C15-C1768.1 (2)
C2-C3-C4-C5型14.9 (2)C13-C14-C15-C1652.9 (2)
C25-C3-C4-C5111.0 (2)C4-C5-C16-C1520.2 (2)
C2-C3-C4-C13型163.35 (15)N1-C5-C16-C15163.31 (15)
C25-C3-C4-C13型70.8 (2)C14-C15-C16-C546.6 (2)
C13-C4-C5-N1172.81 (16)C18-C15-C16-C5164.98 (15)
C3-C4-C5-N15.4 (3)C17-C15-C16-C573.7 (2)
C13-C4-C5-C16型3.5 (3)C1-N1-C19-C20109.2 (2)
C3-C4-C5-C16型178.33 (16)C5-N1-C19-C2080.7 (2)
C1-N1-C5-C46.7 (2)C1-N1-C19-C2468.7 (2)
C19-N1-C5-C4163.63 (17)C5-N1-C19-C24101.5 (2)
C1-N1-C5-C16169.84 (15)C24-C19-C20-C21型1.2 (3)
C19-N1-C5-C1619.8 (2)N1-C19-C20-C21178.97 (17)
C1-C2-C6-O1177.12 (19)C19-C20-C21-C22型1.3 (3)
C3-C2-C6-O14.3 (3)C20-C21-C22-C23型0.2 (3)
C1-C2-C6-C72.1 (2)C21-C22-C23-C241.0 (3)
C3-C2-C6-C7型176.55 (17)C20-C19-C24-C230.0 (3)
O1-C6-C7-C8型2.0 (3)N1-C19-C24-C23型177.89 (17)
C2-C6-C7-C8型178.8 (2)C22-C23-C24-C191.0 (3)
O1-C6-C7-C12型176.25 (18)C2-C3-C25-C2682.6 (2)
C2-C6-C7-C12型2.9 (2)C4-C3-C25-C26型40.4 (2)
C12-C7-C8-C90.5 (3)C3-C25-C26-C2763.6 (2)
C6-C7-C8-C9177.59 (19)C3-C25-C26-C31116.3 (2)
C7-C8-C9-C101.5 (3)C31-C26-C27-C282.5 (3)
C8-C9-C10-C11号机组1.9 (3)C25-C26-C27-C28177.43 (19)
C9-C10-C11-C120.1 (3)C26-C27-C28-C291.7 (3)
C10-C11-C12-C71.9 (3)C27-C28-C29-C300.6 (3)
C10-C11-C12-C1179.68 (19)C28-C29-C30-C311.9 (3)
C8-C7-C12-C11号机组2.2 (3)C29-C30-C31-C26型1.1 (3)
C6-C7-C12-C11176.24 (17)C27-C26-C31-C30型1.2 (3)
C8-C7-C12-C1178.95 (17)C25-C26-C31-C30型178.80 (18)
C6-C7-C12-C12.62 (19)
氢键几何形状(λ,º) 顶部
D类-H(H)···A类D类-H(H)H(H)···A类D类···A类D类-H(H)···A类
C14-H14型B类···氧气0.992.403.337 (2)157
C18-H18型A类···氧气0.982.583.429 (2)145
对称代码:(i)x+3/2,1/2,z(z)+3/2.
 

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