Group 11 complexes of a bulky triazene ligand.
George, Tanner; Grant, Tamika; Munhoz, Isadora Schumann; Do, Thai; Masuda, Jason D.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13107–13118; doi:10.1039/d4dt01561d

data_7716680
_publ_section_title
;
 Group 11 complexes of a bulky triazene ligand.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13107
_journal_page_last               13118
_journal_paper_doi               10.1039/d4dt01561d
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C51 H63 Cl Cu N5, 2(C3 D3)'
_chemical_formula_sum            'C57 H63 Cl Cu D6 N5'
_chemical_formula_weight         929.19
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-03-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-17 deposited with the CCDC.	2024-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.2710(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6515(3)
_cell_length_b                   19.6951(5)
_cell_length_c                   24.8627(7)
_cell_measurement_reflns_used    9212
_cell_measurement_temperature    125
_cell_measurement_theta_max      36.13
_cell_measurement_theta_min      2.65
_cell_volume                     5147.6(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker AXS Inc., 2018)'
_computing_data_reduction        'SAINT V8.40A (Bruker AXS Inc., 2018)'
_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      125
_diffrn_detector                 '100 \\times 140 mm^2^ CMOS sensor'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_detector_type            'Bruker PHOTON III'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       '\k--geometry diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0211
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            239862
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.970
_diffrn_reflns_theta_min         2.227
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\mS 3.0'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.517
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0828 before and 0.0530 after correction.
The Ratio of minimum to maximum transmission is 0.9196.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.796
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     591
_refine_ls_number_reflns         22589
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0437
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+2.0296P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1413
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17921
_reflns_number_total             22589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01561d2.cif
_cod_data_source_block           mo_2022_10_20_jdm_ism_cucl_0m_c
_cod_depositor_comments
'Adding full bibliography for 7716674--7716682.cif.'
_cod_database_code               7716680
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.913
_shelx_estimated_absorpt_t_min   0.840
_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
 C56-C57 = C55-C56 = C57-C55_$1
 1.37 with sigma of 0.001
 C54-C53 = C53-C52
 1.37 with sigma of 0.001
3.a Ternary CH refined with riding coordinates:
 C22(H22), C25(H25), C13(H13), C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B)
3.c Aromatic/amide H refined with riding coordinates:
 C36(H36), C38(H38), C18(H18), C47(H47), C19(H19), C30(H30), C6(H6), C20(H20),
 C8(H8), C45(H45), C32(H32), C7(H7), C31(H31), C52(D52), C53(D53), C54(D54),
 C57(D57), C55(D55), C56(D56)
3.d Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C50(H50A,H50B,H50C), C41(H41A,H41B,
 H41C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C11(H11A,
 H11B,H11C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C49(H49A,H49B,H49C),
 C51(H51A,H51B,H51C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              78108
_shelx_hkl_checksum              17021
_olex2_submission_special_instructions 'No special instructions were received'