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_7711594
_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         'C54 H68 Cl2 Cu4 N6'
_chemical_formula_sum            'C54 H68 Cl2 Cu4 N6'
_chemical_formula_weight         1126.20
_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
_audit_creation_date             2019-07-29
_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                 103.848(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.697(4)
_cell_length_b                   20.986(6)
_cell_length_c                   23.210(7)
_cell_measurement_reflns_used    9901
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.28
_cell_volume                     6005(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1512
_diffrn_reflns_av_unetI/netI     0.1092
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            56373
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.326
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.523
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4099
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       block
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.576
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         10557
_refine_ls_number_restraints     1244
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1642
_refine_ls_R_factor_gt           0.1039
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1826P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2565
_refine_ls_wR_factor_ref         0.3020
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5851
_reflns_number_total             10557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02654f2.cif
_cod_data_source_block           1_a
_cod_database_code               7711594
_shelx_shelxl_version_number     2018/3
_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
 C53-C52 = C52-C51 = C50-C49 = C43-C38 = C44-C43 = C45-C43 = C47-C46 = C21-C19
 = C20-C19 = C19-C15 = C17-C16 = C23-C22 = C27-C26 = C25-C24
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C38 \\sim C4 \\sim C46 \\sim C17 \\sim C20 \\sim C22 \\sim C34 \\sim C5 \\sim
C32 \\sim C16 \\sim C7 \\sim C39 \\sim C43 \\sim C50 \\sim C33 \\sim C40 \\sim
C41 \\sim C14 \\sim C44 \\sim C6 \\sim C51 \\sim C21 \\sim C12 \\sim C54 \\sim
C23 \\sim C13 \\sim C27 \\sim C53 \\sim C47 \\sim C48 \\sim C24 \\sim C18 \\sim
C52 \\sim C25 \\sim C26 \\sim C45 \\sim C9 \\sim C30 \\sim C2 \\sim C36 \\sim
C35 \\sim C8 \\sim C29 \\sim C37 \\sim C28 \\sim C3 \\sim C1 \\sim C10 \\sim
C49 \\sim C15 \\sim C42 \\sim C11 \\sim C31 \\sim C19: within 3.8A with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq, Uanis(Cu1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(Cl2) \\sim Ueq, Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
4.a Ternary CH refined with riding coordinates:
 C46(H46), C16(H16), C43(H43), C19(H19)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C50(H50A,H50B), C51(H51A,H51B), C54(H54A,H54B), C23(H23A,
 H23B), C27(H27A,H27B), C53(H53A,H53B), C24(H24A,H24B), C52(H52A,H52B),
 C25(H25A,H25B), C26(H26A,H26B), C49(H49A,H49B)
4.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C34(H34), C5(H5), C32(H32), C7(H7), C39(H39), C33(H33), C40(H40),
 C41(H41), C14(H14), C6(H6), C12(H12), C13(H13), C9(H9), C36(H36), C31(H31)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C44(H44A,H44B,H44C), C21(H21A,H21B,
 H21C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C18(H18A,H18B,H18C), C45(H45A,
 H45B,H45C)
;
_shelx_res_checksum              2113
_shelx_hkl_checksum              75772
_shelx_fab_checksum              3440
_olex2_submission_special_instructions 'No special instructions were received'