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_7711596
_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_absolute_configuration unk
_chemical_formula_moiety         'C56 H72 Cu4 I2 N6, 1.02[C7H8]'
_chemical_formula_sum            'C56 H72 Cu4 I2 N6'
_chemical_formula_weight         1337.15
_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             2021-04-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-01-18 deposited with the CCDC.	2022-10-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.382(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.7379(12)
_cell_length_b                   11.7973(6)
_cell_length_c                   12.4396(7)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      30.113
_cell_measurement_theta_min      2.747
_cell_volume                     3137.9(3)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (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 0.997
_diffrn_measured_fraction_theta_max 0.962
_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  0.0577
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            61272
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.875
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.353
_diffrn_reflns_theta_min         2.747
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.2899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1246 before and 0.0715 after correction.
The Ratio of minimum to maximum transmission is 0.3884.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       block
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details
;
 Flack x determined using 2875 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.014(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         9825
_refine_ls_number_restraints     559
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+2.3064P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0797
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    0.941
_reflns_Friedel_fraction_max     0.781
_reflns_number_gt                7638
_reflns_number_total             9825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02654f2.cif
_cod_data_source_block           20210428b_sq
_cod_database_code               7711596
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.798
_shelx_estimated_absorpt_t_min   0.719
_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. Shared sites
{C16, C16A}
3. Restrained distances
 C27A-C25A = C25A-C26A
 1.54 with sigma of 0.02
 C24A-C22A = C22A-C23A
 1.54 with sigma of 0.02
 C27A-C26A
 2.515 with sigma of 0.04
 C24A-C23A
 2.515 with sigma of 0.04
4. Uiso/Uaniso restraints and constraints
C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim
C24 \\sim C25 \\sim C26 \\sim C27 \\sim C16A \\sim C17A \\sim C18A \\sim C19A
\\sim C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C25A \\sim C26A
\\sim C27A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.01
within 2A
Uanis(C16) = Uanis(C16A)
5. Rigid body (RIGU) restrains
 C16, C24, C22, C17, C26, C18, C23, C19, C25, C20, C27, C21, N3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C16A, C24A, C22A, C17A, C26A, C18A, C23A, C19A, C25A, C20A, C27A, C21A, N3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Sof(C16A)=Sof(C17A)=Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19A)=Sof(C20A)=
 Sof(H20A)=Sof(C21A)=Sof(C22A)=Sof(H22A)=Sof(C23A)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25A)=Sof(H25A)=
 Sof(C26A)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=1-FVAR(1)
 Sof(C16)=Sof(C17)=Sof(C18)=Sof(H18)=Sof(C19)=Sof(H19)=Sof(C20)=Sof(H20)=
 Sof(C21)=Sof(C22)=Sof(H22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=
 Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=
 Sof(H26C)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C22A(H22A), C25A(H25A)
7.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)
7.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C007(H007), C7(H7), C18(H18), C19(H19), C20(H20),
 C18A(H18A), C19A(H19A), C20A(H20A)
7.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C23A(H23D,H23E,H23F), C24A(H24D,H24E,H24F), C26A(H26D,H26E,H26F),
 C27A(H27D,H27E,H27F)
;
_shelx_res_checksum              70141
_shelx_hkl_checksum              48925
_shelx_fab_checksum              64099
_platon_squeeze_special_details
;
A solvent mask was calculated and 108 electrons were 
found in a volume of 482\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
1.02[C7H8] per Asymmetric Unit 
which account for 102 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'