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_4128040
_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 H75 Cu3 N15, 4(B F4), 2.25(O), C H4 O'
_chemical_formula_sum            'C46 H79 B4 Cu3 F16 N15 O3.25'
_chemical_formula_weight         1432.10
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 103.463(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4103(12)
_cell_length_b                   23.0536(15)
_cell_length_c                   15.5199(10)
_cell_measurement_reflns_used    9644
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.76
_cell_measurement_theta_min      2.22
_cell_volume                     6406.0(7)
_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      100.03
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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  0.0540
_diffrn_reflns_av_unetI/netI     0.0304
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            140570
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.154
_diffrn_reflns_theta_min         2.147
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6385
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0948 before and 0.0564 after correction.
The Ratio of minimum to maximum transmission is 0.8565.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       plate
_exptl_crystal_F_000             2948
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.888
_refine_diff_density_min         -3.088
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         14169
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1023
_refine_ls_R_factor_gt           0.0839
_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^)+(0.1594P)^2^+27.1648P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2508
_refine_ls_wR_factor_ref         0.2646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11028
_reflns_number_total             14169
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b04822_si_002.cif
_cod_data_source_block           y_a_sq_s
_cod_database_code               4128040
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O2A-O2
 1.42 with sigma of 0.01
 O2-O2A
 1.42 with sigma of 0.01
 B4-F13 \\sim B4-F14 \\sim B4-F15 \\sim B4-F16
 with sigma of 0.02
 B4'-F13' \\sim B4'-F14' \\sim B4'-F15' \\sim B4'-F16'
 with sigma of 0.02
 F13-F14 \\sim F13-F15 \\sim F13-F16 \\sim F14-F15 \\sim F14-F16 \\sim F15-F16
 with sigma of 0.02
 F13'-F14' \\sim F13'-F15' \\sim F13'-F16' \\sim F14'-F15' \\sim F14'-F16'
\\sim F15'-F16'
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O3A) \\sim Ueq, Uanis(O2A)
\\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.005
4. Others
 Sof(B4')=Sof(F13')=Sof(F14')=Sof(F15')=Sof(F16')=1-FVAR(1)
 Sof(F13)=Sof(F14)=Sof(F15)=Sof(F16)=Sof(B4)=FVAR(1)
 Fixed Sof: O2(0.5) O2A(0.5) O3(0.6) O3A(0.4) O4(0.25)
5.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)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), N5(H5), N6(H6), C2(H2A), C5(H5A), C8(H8),
 C11(H11), C14(H14), C17(H17)
5.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), C46(H46A,H46B,H46C)
5.d Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_shelx_res_checksum              6540
_shelx_hkl_checksum              71962
_shelx_fab_checksum              83967
_olex2_submission_special_instructions 'No special instructions were received'