Crystal structure of 1,1′-diformyl-4,4′-(6H,12H-5,11-methano-dibenzo[b,f][11,5]diazocine-2,8-diyl)dibenzene, C29H22N2O2
Qiu, Feng; Wan, Yu; Huang, Shu-ying; Zhou, Qiu-ju; Cui, Hao; Chu, Yan-huan; Zhou, Sheng-Liang; Han, Xiang-en; Wu, Hui; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 569–572; doi:10.1515/ncrs-2015-0193

data_8106942
_publ_section_title
;
 Crystal structure of
 1,1&#x2032;-diformyl-4,4&#x2032;-(6H,12H-5,11-methano-dibenzo[b,f][11,5]diazocine-2,8-diyl)dibenzene,
 C29H22N2O2
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              569
_journal_page_last               572
_journal_paper_doi               10.1515/ncrs-2015-0193
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C29 H22 N2 O2'
_chemical_formula_sum            'C29 H22 N2 O2'
_chemical_formula_weight         430.48
_chemical_name_systematic
;
1,1'-diformyl-4,4'-(6<i>H</i>,12<i>H</i>-5,11-methano-
dibenzo[<i>b</i>,<i>f</i>][<i>1</i>1,<i>5</i>]diazocine-2,8-diyl)dibenzene
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 115.9410(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.4995(6)
_cell_length_b                   9.9370(3)
_cell_length_c                   21.6466(6)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      26.340
_cell_measurement_theta_min      2.301
_cell_volume                     4352.1(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            37098
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.585
_diffrn_reflns_theta_min         1.006
_exptl_absorpt_coefficient_mu    0.083
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0547 before and 0.0409 after correction.
The Ratio of minimum to maximum transmission is 0.8602.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       block
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.037
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     605
_refine_ls_number_reflns         9973
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+0.8609P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1213
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6707
_reflns_number_total             9973
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2015-0193_suppl.cif
_cod_data_source_block           exp_266_109
_cod_database_code               8106942
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Rigid bond restraints
 O4, C64, C39, C55
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3. Others
 Sof(H64A)=Sof(O4A)=1-FVAR(1)
 Sof(H64)=Sof(O4)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C42(H42A,H42B), C51(H51A,H51B), C44(H44A,H44B), C49(H49A,
 H49B), C52(H52A,H52B)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C10(H10), C11(H11), C12(H12), C26(H26), C27(H27), C32(H32),
 C38(H38), C46(H46), C48(H48), C56(H56), C57(H57), C59(H59), C61(H61), C64(H64),
  C64(H64A), C20(H20), C21(H21), C22(H22), C23(H23), C31(H31), C36(H36),
 C41(H41), C43(H43), C47(H47), C50(H50), C54(H54), C55(H55), C58(H58), C60(H60),
  C63(H63), C66(H66)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'