Triphenylene-Bridged Trinuclear Complexes of Cu: Models for Spin Interactions in Two-Dimensional Electrically Conductive Metal-Organic Frameworks.
Yang, Luming; He, Xin; Dincă, Mircea; Journal of the American Chemical Society 141 (2019) 10475–10480; doi:10.1021/jacs.9b04822

data_4128041
_publ_section_title
;
 Triphenylene-Bridged Trinuclear Complexes of Cu: Models for Spin
 Interactions in Two-Dimensional Electrically Conductive Metal-Organic
 Frameworks.
;
_journal_issue                   26
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10475
_journal_page_last               10480
_journal_paper_doi               10.1021/jacs.9b04822
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C45 H69 Cu3 N9 O6, 0.5(C2 H4 Cl2), 3(B F4)'
_chemical_formula_sum            'C46 H71 B3 Cl Cu3 F12 N9 O6'
_chemical_formula_weight         1332.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-02-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                83.698(2)
_cell_angle_beta                 80.855(2)
_cell_angle_gamma                68.665(2)
_cell_formula_units_Z            4
_cell_length_a                   16.8057(12)
_cell_length_b                   17.2937(11)
_cell_length_c                   24.2896(15)
_cell_measurement_reflns_used    9073
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.75
_cell_measurement_theta_min      2.62
_cell_volume                     6481.6(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            260400
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.188
_diffrn_reflns_theta_min         2.063
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6574
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1089 before and 0.0582 after correction.
The Ratio of minimum to maximum transmission is 0.8818.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       needle
_exptl_crystal_F_000             2740
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.175
_refine_diff_density_min         -1.467
_refine_diff_density_rms         0.120
_refine_ls_extinction_coef       0.00051(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1543
_refine_ls_number_reflns         28760
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0743
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0961P)^2^+14.2955P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23085
_reflns_number_total             28760
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04822_si_001.cif
_cod_data_source_block           y_a_sq_s
_cod_database_code               4128041
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 B6-F21 \\sim B6-F22 \\sim B6-F23 \\sim B6-F24
 with sigma of 0.02
 F21-F22 \\sim F21-F23 \\sim F21-F24 \\sim F22-F23 \\sim F22-F24 \\sim F23-F24
 with sigma of 0.02
 B6-F21A \\sim B6-F22A \\sim B6-F23A \\sim B6-F24A
 with sigma of 0.02
 F21A-F22A \\sim F21A-F23A \\sim F21A-F24A \\sim F22A-F23A \\sim F22A-F24A
\\sim F23A-F24A
 with sigma of 0.02
 B5-F17 \\sim B5-F18 \\sim B5-F19 \\sim B5-F20
 with sigma of 0.02
 F17-F18 \\sim F17-F19 \\sim F17-F20 \\sim F18-F19 \\sim F18-F20 \\sim F19-F20
 with sigma of 0.02
 B5A-F17A \\sim B5A-F18A \\sim B5A-F19A \\sim B5A-F20A
 with sigma of 0.02
 F17A-F18A \\sim F17A-F19A \\sim F17A-F20A \\sim F18A-F19A \\sim F18A-F20A
\\sim F19A-F20A
 with sigma of 0.02
3. Others
 Sof(F21A)=Sof(F22A)=Sof(F23A)=Sof(F24A)=1-FVAR(1)
 Sof(F21)=Sof(F22)=Sof(F23)=Sof(F24)=FVAR(1)
 Sof(B5A)=Sof(F17A)=Sof(F18A)=Sof(F19A)=Sof(F20A)=1-FVAR(2)
 Sof(F17)=Sof(F18)=Sof(F19)=Sof(F20)=Sof(B5)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C21(H21A,H21B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,
 H26B), C27(H27A,H27B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B),
 C33(H33A,H33B), C35(H35A,H35B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B),
  C41(H41A,H41B), C42(H42A,H42B), C44(H44A,H44B), C45(H45A,H45B), C65(H65A,
 H65B), C66(H66A,H66B), C68(H68A,H68B), C69(H69A,H69B), C71(H71A,H71B),
 C72(H72A,H72B), C74(H74A,H74B), C75(H75A,H75B), C77(H77A,H77B), C78(H78A,H78B),
  C80(H80A,H80B), C81(H81A,H81B), C83(H83A,H83B), C84(H84A,H84B), C86(H86A,
 H86B), C87(H87A,H87B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B),
 C92(H92A,H92B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C5(H5), C8(H8), C11(H11), C14(H14), C17(H17), C47(H47), C50(H50),
 C53(H53), C56(H56), C59(H59), C62(H62)
4.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C28(H28A,H28B,
 H28C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C37(H37A,H37B,H37C), C40(H40A,
 H40B,H40C), C43(H43A,H43B,H43C), C64(H64A,H64B,H64C), C67(H67A,H67B,H67C),
 C70(H70A,H70B,H70C), C73(H73A,H73B,H73C), C76(H76A,H76B,H76C), C79(H79A,H79B,
 H79C), C82(H82A,H82B,H82C), C85(H85A,H85B,H85C), C88(H88A,H88B,H88C)
;
_shelx_res_checksum              88891
_shelx_hkl_checksum              49222
_shelx_fab_checksum              15494
_olex2_submission_special_instructions 'No special instructions were received'