Crystal structure of diethyl 1,9-bis(4-fluorophenyl)-4,6-diphenylhexahydro-3H-2,7,3,5-(epimethanetriyliminomethanetriyl)cyclopenta [b]pyridine-3,7(2H)-dicarboxylate, C40H36F2N2O4
Zhang, Zi-Ang; Li, Jun-Xiang; Lu, Sen-Bao; Li, Peng; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 1185–1187; doi:10.1515/ncrs-2023-0388

data_8107697
_publ_section_title
;
 Crystal structure of diethyl
 1,9-bis(4-fluorophenyl)-4,6-diphenylhexahydro-3H-2,7,3,5-(epimethanetriyliminomethanetriyl)cyclopenta
 [b]pyridine-3,7(2H)-dicarboxylate, C40H36F2N2O4
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1185
_journal_page_last               1187
_journal_paper_doi               10.1515/ncrs-2023-0388
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C40 H36 F2 N2 O4'
_chemical_formula_sum            'C40 H36 F2 N2 O4'
_chemical_formula_weight         646.71
_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                 102.353(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8180(16)
_cell_length_b                   19.355(3)
_cell_length_c                   17.930(3)
_cell_measurement_reflns_used    4017
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.51
_cell_measurement_theta_min      2.33
_cell_volume                     3328.3(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20489
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         1.568
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.221
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.041
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         7585
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.1046
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1561
_refine_ls_wR_factor_ref         0.1866
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4295
_reflns_number_total             7585
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0388_suppl_001.cif
_cod_data_source_block           1
_cod_database_code               8107697
_shelx_estimated_absorpt_t_max   0.987
_shelx_estimated_absorpt_t_min   0.984
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H1(0.092) H2(0.104) H4(0.117) H5(0.102) H7(0.089) H8(0.1)
 H9(0.108) H17(0.064) H16(0.061) H15(0.057) H13(0.065) H20(0.059) H18(0.063)
 H21(0.059) H26(0.092) H25(0.092) H24(0.086) H23(0.074) H27(0.078) H32(0.071)
 H31(0.087) H29(0.096) H28(0.077) H36A(0.256) H36B(0.256) H36C(0.256)
 H38A(0.08) H38B(0.08) H39A(0.194) H39B(0.194) H39C(0.194) H38C(0.08)
 H38D(0.08) H39D(0.171) H39E(0.171) H39F(0.171) H35A(0.105) H35B(0.105)
 H11B(0.09) H10B(0.094) H10A(0.098) H11A(0.085) H40(0.063)
 Fixed X: H1(0.562781) H2(0.702761) H4(0.978888) H5(0.834204) H7(0.506494)
 H8(0.649528) H9(0.88978) H17(0.362804) H16(0.281579) H15(0.456343)
 H13(0.525529) H20(0.530858) H18(0.413455) H21(0.718442) H26(0.113357) H25(-
 0.051169) H24(-0.076096) H23(0.064398) H27(0.250714) H32(0.636321)
 H31(0.728432) H29(0.542306) H28(0.445575) H36A(0.804493) H36B(0.649624)
 H36C(0.731292) H38A(0.128871) H38B(0.249765) H39A(0.051118) H39B(0.115586)
 H39C(-0.009363) H38C(0.188204) H38D(0.224898) H39D(-0.007007) H39E(0.017365)
 H39F(-0.019139) H35A(0.796102) H35B(0.87708) H11B(0.806562) H10B(0.948072)
 H10A(0.979747) H11A(0.836696) H40(0.198989)
 Fixed Y: H1(0.474591) H2(0.432216) H4(0.578119) H5(0.625064) H7(0.419474)
 H8(0.325738) H9(0.345286) H17(0.510689) H16(0.606945) H15(0.683123)
 H13(0.547136) H20(0.723768) H18(0.533521) H21(0.660852) H26(0.861676)
 H25(0.860493) H24(0.763119) H23(0.66886) H27(0.766017) H32(0.807797)
 H31(0.913232) H29(0.896424) H28(0.793381) H36A(0.748746) H36B(0.725914)
 H36C(0.764866) H38A(0.56726) H38B(0.615422) H39A(0.678473) H39B(0.711697)
 H39C(0.659859) H38C(0.692503) H38D(0.619266) H39D(0.640663) H39E(0.577878)
 H39F(0.650733) H35A(0.635055) H35B(0.674027) H11B(0.527787) H10B(0.431634)
 H10A(0.448273) H11A(0.543352) H40(0.605594)
 Fixed Z: H1(0.194619) H2(0.1188) H4(0.190126) H5(0.262903) H7(0.385721)
 H8(0.39376) H9(0.412287) H17(0.3593) H16(0.413771) H15(0.46544) H13(0.470127)
 H20(0.261509) H18(0.2408) H21(0.333591) H26(0.23132) H25(0.306016)
 H24(0.376693) H23(0.374222) H27(0.226917) H32(0.308344) H31(0.355312)
 H29(0.530331) H28(0.483801) H36A(0.679328) H36B(0.647965) H36C(0.594538)
 H38A(0.051306) H38B(0.035666) H39A(-0.008512) H39B(0.070938) H39C(0.063107)
 H38C(0.051094) H38D(0.022386) H39D(-0.016849) H39E(0.039682) H39F(0.068241)
 H35A(0.65384) H35B(0.599958) H11B(0.503928) H10B(0.509432) H10A(0.433165)
 H11A(0.43157) H40(0.278819)
;
_shelx_res_checksum              75862
_shelx_hkl_checksum              15784
_shelx_shelxl_version_number     2016/6
_olex2_submission_special_instructions 'No special instructions were received'