Halide-Bridged Tetranuclear Organocopper(I) Clusters Supported by the Indolyl-based NCN Pincer Ligands and Their Catalytic Activities towards Hydrophosphination of Alkenes
Yuan, Qingbing; Huang, Zeming; Wu, weikang; Hong, Dongjing; Zhu, Shan; Wei, Jieding; Zhou, Shuangliu; Wang, Shaowu; Dalton Transactions  (2022) –; doi:10.1039/D2DT02654F

data_7711595
_publ_section_title
;
 Halide-Bridged Tetranuclear Organocopper(I) Clusters Supported by the
 Indolyl-based NCN Pincer Ligands and Their Catalytic Activities towards
 Hydrophosphination of Alkenes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02654F
_journal_year                    2022
_chemical_formula_moiety         'C56 H72 Br2 Cu4 N6'
_chemical_formula_sum            'C56 H72 Br2 Cu4 N6'
_chemical_formula_weight         1243.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-11-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-01-18 deposited with the CCDC.	2022-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.044(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.510(3)
_cell_length_b                   11.7559(14)
_cell_length_c                   12.4242(14)
_cell_measurement_reflns_used    7392
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.41
_cell_measurement_theta_min      2.48
_cell_volume                     3093.6(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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 1.000
_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  0.0337
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17740
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.469
_diffrn_reflns_theta_min         1.665
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.685
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3265
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.335
_exptl_crystal_description       block
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.244(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         7002
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0594
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.064
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0592P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1061
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.982
_reflns_number_gt                5558
_reflns_number_total             7002
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02654f2.cif
_cod_data_source_block           1_a_CCDC1
_cod_database_code               7711595
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.616
_shelx_estimated_absorpt_t_min   0.590
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.756(15)
 0.244(15)
2. 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
3. Rigid bond restraints
 C16, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C12) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C17)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq:
with sigma of 0.001 and sigma for terminal atoms of 0.002
5.a Ternary CH refined with riding coordinates:
 C16(H16), C19(H19)
5.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C24(H24A,H24B), C22(H22A,H22B), C23(H23A,H23B), C28(H28A,
 H28B), C25(H25A,H25B), C26(H26A,H26B)
5.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C4(H4), C7(H7), C14(H14), C6(H6), C5(H5), C12(H12), C13(H13)
5.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C18(H18A,H18B,H18C), C17(H17A,H17B,H17C), C20(H20A,H20B,
 H20C)
;
_shelx_res_checksum              18579
_shelx_hkl_checksum              83568
_shelx_fab_checksum              34266
_olex2_submission_special_instructions 'No special instructions were received'