Nickel-catalyzed synthesis of Zn(i)–Zn(i) bonded compounds
Jiang, Shengjie; Cai, Yanping; Carpentier, Ambre; del Rosal, Iker; Maron, Laurent; Xu, Xin; Chemical Communications  (2021) –; doi:10.1039/D1CC05719G

data_7129302
_publ_section_title
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 Nickel-catalyzed synthesis of Zn(i)--Zn(i) bonded compounds
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05719G
_journal_year                    2021
_chemical_formula_moiety         'C62 H76 N4 P2 Zn2, C7 H8'
_chemical_formula_sum            'C69 H84 N4 P2 Zn2'
_chemical_formula_weight         1162.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-10
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                103.7740(10)
_cell_angle_beta                 93.3920(10)
_cell_angle_gamma                114.9870(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5584(5)
_cell_length_b                   13.8088(5)
_cell_length_c                   21.0026(9)
_cell_measurement_reflns_used    9962
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      27.40
_cell_measurement_theta_min      2.19
_cell_volume                     3153.1(2)
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0677
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            108875
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.527
_diffrn_reflns_theta_min         2.239
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.854
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6533
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1102 before and 0.0725 after correction. The Ratio of minimum to maximum transmission is 0.8762. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.375
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         14487
_refine_ls_number_restraints     136
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0711
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0584P)^2^+6.2350P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1448
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11444
_reflns_number_total             14487
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05719g2.cif
_cod_data_source_block           Complex_2a
_cod_database_code               7129302
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.919
_shelx_estimated_absorpt_t_min   0.861
_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
 C63-C64
 1.51 with sigma of 0.02
 C64-C65 = C64-C69 = C66-C67
 1.39 with sigma of 0.02
 C65-C66 = C67-C68 = C68-C69
 1.38 with sigma of 0.02
 C64-C66
 2.42 with sigma of 0.04
 C65-C67
 2.39 with sigma of 0.04
 C64-C68
 2.41 with sigma of 0.04
 C66-C68 = C67-C69
 2.4 with sigma of 0.04
 C63-C65 = C63-C69
 2.52 with sigma of 0.04
 C64-C65 \\sim C65-C66 \\sim C66-C67 \\sim C67-C68 \\sim C68-C69 \\sim C69-C64
 with sigma of 0.02
 C64-C68 \\sim C64-C66 \\sim C69-C67 \\sim C65-C69 \\sim C66-C68 \\sim C65-C67
 with sigma of 0.04
 C63-C69 \\sim C63-C65
 with sigma of 0.04
3. Restrained planarity
 C63, C64, C65, C66, C67, C68, C69
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C68 \\sim C69: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A
5. Rigid body (RIGU) restrains
 C63, C64, C65, C66, C67, C68, C69
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 C26(H26), C29(H29), C57(H57), C60(H60)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C37(H37A,H37B), C38(H38A,H38B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C22(H22), C23(H23), C24(H24), C34(H34), C40(H40),
  C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48),
 C49(H49), C50(H50), C53(H53), C54(H54), C55(H55), C65(H65), C66(H66), C67(H67),
  C68(H68), C69(H69)
6.d Fitted hexagon refined as free rotating group:
 C64(C65,C66,C67,C68,C69)
6.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C36(H36A,H36B,
 H36C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C61(H61A,H61B,H61C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C)
;
_shelx_res_checksum              11478
_olex2_submission_special_instructions 'No special instructions were received'