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_7711599
_publ_section_title
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 Halide-Bridged Tetranuclear Organocopper(I) Clusters Supported by the
 Indolyl-based NCN Pincer Ligands and Their Catalytic Activities towards
 Hydrophosphination of Alkenes
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_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02654F
_journal_year                    2022
_chemical_formula_moiety         'C56 H72 Cl2 Cu4 N6, 0.825[C4H8O]'
_chemical_formula_sum            'C56 H72 Cl2 Cu4 N6'
_chemical_formula_weight         1154.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-29
_audit_creation_method
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Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
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_audit_update_record
;
2022-01-18 deposited with the CCDC.	2022-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.2010(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.1754(12)
_cell_length_b                   12.3278(7)
_cell_length_c                   44.251(2)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      24.41
_cell_measurement_theta_min      2.21
_cell_volume                     11823.8(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.990
_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  0.0719
_diffrn_reflns_av_unetI/netI     0.0651
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            136059
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.467
_diffrn_reflns_theta_min         1.136
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.548
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.3221
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1182 before and 0.0581 after correction.
The Ratio of minimum to maximum transmission is 0.4320.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       block
_exptl_crystal_F_000             4800
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1241
_refine_ls_number_reflns         26767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0967
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+2.9351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1152
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15891
_reflns_number_total             26767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02654f2.cif
_cod_data_source_block           210514b
_cod_original_cell_volume        11823.9(11)
_cod_database_code               7711599
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.757
_shelx_estimated_absorpt_t_min   0.727
_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.a Ternary CH refined with riding coordinates:
 C23(H23), C26(H26), C51(H51), C54(H54), C79(H79), C82(H82), C107(H107),
 C110(H110)
2.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B),
 C14(H14A,H14B), C15(H15A,H15B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C65(H65A,
 H65B), C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B),
 C70(H70A,H70B), C71(H71A,H71B), C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B),
  C96(H96A,H96B), C97(H97A,H97B), C98(H98A,H98B), C99(H99A,H99B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C16(H16), C19(H19), C20(H20), C21(H21),
 C32(H32), C33(H33), C34(H34), C35(H35), C44(H44), C47(H47), C48(H48), C49(H49),
  C60(H60), C61(H61), C62(H62), C63(H63), C72(H72), C75(H75), C76(H76),
 C77(H77), C88(H88), C89(H89), C90(H90), C91(H91), C100(H100), C103(H103),
 C104(H104), C105(H105)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C80(H80A,H80B,H80C), C81(H81A,H81B,H81C), C83(H83A,H83B,H83C),
 C84(H84A,H84B,H84C), C108(H10C,H10D,H10E), C109(H10F,H10G,H10H), C111(H11C,
 H11D,H11E), C112(H11F,H11G,H11H)
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_smtbx_masks_special_details
;
A solvent mask was calculated and 264 electrons were 
found in a volume of 1948\%A^3^ in 4 voids per unit cell. 
This is consistent with the presence of 
0.06[C4H8O] per Asymmetric Unit 
which account for 264 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74192
_shelx_hkl_checksum              49803
_shelx_fab_checksum              18865
_olex2_submission_special_instructions 'No special instructions were received'