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_7129296
_publ_section_title
;
 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         'C25 H43 N2 P Zn'
_chemical_formula_sum            'C25 H43 N2 P Zn'
_chemical_formula_weight         467.95
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-09-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-27 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.562(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8843(11)
_cell_length_b                   10.2159(5)
_cell_length_c                   15.6744(9)
_cell_measurement_reflns_used    6769
_cell_measurement_temperature    223
_cell_measurement_theta_max      28.9900
_cell_measurement_theta_min      3.2120
_cell_volume                     2604.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      223
_diffrn_detector_area_resol_mean 10.4471
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_details
;
  1 omega  -67.00   48.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8077  -19.0000  -60.0000 115

  2 omega   12.00   55.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8077  -99.0000  -30.0000 43

  3 omega  -12.00   15.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       13.8077  -38.0000  -90.0000 27

  4 omega   19.00   46.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5889   38.0000  -30.0000 27

  5 omega -105.00  -57.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -14.5889 -178.0000   90.0000 48
;
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0259551000
_diffrn_orient_matrix_UB_12      -0.0263152000
_diffrn_orient_matrix_UB_13      0.0443944000
_diffrn_orient_matrix_UB_21      0.0204684000
_diffrn_orient_matrix_UB_22      0.0610268000
_diffrn_orient_matrix_UB_23      0.0130882000
_diffrn_orient_matrix_UB_31      -0.0284366000
_diffrn_orient_matrix_UB_32      0.0200389000
_diffrn_orient_matrix_UB_33      0.0182642000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0369
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            17437
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.237
_diffrn_reflns_theta_min         2.914
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         6825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0475P)^2^+0.6644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1073
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5260
_reflns_number_total             6825
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05719g2.cif
_cod_data_source_block           Complex_1c
_cod_database_code               7129296
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N P Zn'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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), C20(H20), C8(H8), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C6(H6A,H6B)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C16(H16), C17(H17), C3(H3)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C25(H25A,H25B,H25C), C24(H24A,H24B,H24C),
 C9(H9A,H9B,H9C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C10(H10A,H10B,H10C),
  C13(H13A,H13B,H13C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              56786
_olex2_submission_special_instructions 'No special instructions were received'