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_7711597
_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 Cu4 I2 N6'
_chemical_formula_sum            'C54 H68 Cu4 I2 N6'
_chemical_formula_weight         1309.10
_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             2019-08-28
_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                 95.409(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.426(11)
_cell_length_b                   11.631(13)
_cell_length_c                   44.05(4)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    273(2)
_cell_measurement_theta_max      24.51
_cell_measurement_theta_min      2.97
_cell_volume                     6338(11)
_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)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.982
_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  0.0909
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_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            103003
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.647
_diffrn_reflns_theta_min         2.909
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5302
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_description       block
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.392
_refine_diff_density_min         -1.978
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     603
_refine_ls_number_reflns         14523
_refine_ls_number_restraints     1255
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1568
_refine_ls_R_factor_gt           0.1039
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0714P)^2^+88.0142P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2178
_refine_ls_wR_factor_ref         0.2387
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8887
_reflns_number_total             14523
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02654f2.cif
_cod_data_source_block           1_a_CCDC2
_cod_database_code               7711597
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.653
_shelx_estimated_absorpt_t_min   0.628
_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
 C52-C51 = C53-C52 = C54-C53 = C25-C24
 1.54 with sigma of 0.005
 C26-C25 = C27-C26
 1.54 with sigma of 0.01
 H50B-H51B
 2 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C9 \\sim C2 \\sim C36 \\sim C29 \\sim C37 \\sim C10 \\sim C15 \\sim C3
\\sim C8 \\sim C28 \\sim C30 \\sim C11 \\sim C42 \\sim C22 \\sim C35 \\sim C49
\\sim C34 \\sim C19 \\sim C38 \\sim C46 \\sim C4 \\sim C33 \\sim C43 \\sim C14
\\sim C16 \\sim C6 \\sim C23 \\sim C32 \\sim C50 \\sim C39 \\sim C5 \\sim C31
\\sim C54 \\sim C7 \\sim C12 \\sim C24 \\sim C41 \\sim C13 \\sim C40 \\sim C51
\\sim C18 \\sim C21 \\sim C20 \\sim C27 \\sim C17 \\sim C45 \\sim C47 \\sim C48
\\sim C44 \\sim C25 \\sim C53 \\sim C52 \\sim C26: within 3.8A with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Ternary CH refined with riding coordinates:
 C19(H19), C46(H46), C43(H43), C16(H16)
4.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C49(H49A,H49B), C23(H23A,H23B), C50(H50A,H50B), C54(H54A,
 H54B), C24(H24A,H24B), C51(H51A,H51B), C27(H27A,H27B), C25(H25A,H25B),
 C53(H53A,H53B), C52(H52A,H52B), C26(H26A,H26B)
4.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C36(H36), C34(H34), C4(H4), C33(H33), C14(H14), C6(H6), C32(H32),
 C39(H39), C5(H5), C31(H31), C7(H7), C12(H12), C41(H41), C13(H13), C40(H40)
4.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C20(H20A,H20B,H20C), C17(H17A,H17B,
 H17C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C44(H44A,
 H44B,H44C)
;
_shelx_res_checksum              19269
_shelx_hkl_checksum              34110
_shelx_fab_checksum              5427
_olex2_submission_special_instructions 'No special instructions were received'