Heteronuclear assembly of Ni‒Cu dithiolato complexes: synthesis, structures, and reactivity studies
Chu, Xiaoxiao; Xu, Xin; Su, Hao; Raje, Sakthi; Angamuthu, Raja; Tung, Chen-Ho; Wang, Wenguang; Inorganic Chemistry Frontiers 4 (2017) 706–; doi:10.1039/C6QI00536E

data_4349640
_publ_section_title
;
 Heteronuclear assembly of Ni--Cu dithiolato complexes: synthesis,
 structures, and reactivity studies
;
_journal_issue                   4
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              706
_journal_paper_doi               10.1039/C6QI00536E
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         'C58 H60 Ag2 Ni2 P4 S4, 2(B F4)'
_chemical_formula_sum            'C58 H60 Ag2 B2 F8 Ni2 P4 S4'
_chemical_formula_weight         1515.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-11-26 deposited with the CCDC.
2017-02-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.577(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.906(2)
_cell_length_b                   11.5072(6)
_cell_length_c                   19.2841(10)
_cell_measurement_reflns_used    7993
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.613
_cell_measurement_theta_min      2.542
_cell_volume                     6728.9(7)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0780
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28546
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.539
_exptl_absorpt_coefficient_mu    1.400
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       solid
_exptl_crystal_F_000             3056
_refine_diff_density_max         1.192
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5919
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0613
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+102.1220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4131
_reflns_number_total             5919
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00536e2.cif
_cod_data_source_block           p
_cod_original_cell_volume        6728.8(7)
_cod_database_code               4349640
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
F0AA \\sim F1 \\sim F2 \\sim F4 \\sim F6 \\sim F7 \\sim F9 \\sim B5: within
1.7A with sigma of 0.002 and sigma for terminal atoms of 0.08
C58: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
3. Others
 Fixed Sof: F0AA(0.5) F2(0.5) F4(0.5) F6(0.5) F7(0.5) F9(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C14(H14A,H14B), C27(H27A,H27B), C29(H29A,H29B), C58(H58A,H58B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11),
 C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C22(H22), C23(H23),
  C24(H24), C25(H25), C26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'