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_4349638
_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         'C55 H54 Cu Ni P4 S2, 2(C2 H3 N), B F4'
_chemical_formula_sum            'C59 H60 B Cu F4 N2 Ni P4 S2'
_chemical_formula_weight         1194.15
_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
_audit_creation_date             2016-05-26
_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                87.047(4)
_cell_angle_beta                 81.675(4)
_cell_angle_gamma                66.275(3)
_cell_formula_units_Z            2
_cell_length_a                   12.202(5)
_cell_length_b                   12.646(5)
_cell_length_c                   19.879(8)
_cell_measurement_reflns_used    3133
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.491
_cell_measurement_theta_min      2.577
_cell_volume                     2778.6(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0722
_diffrn_reflns_av_unetI/netI     0.0961
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25625
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.575
_exptl_absorpt_coefficient_mu    0.966
_exptl_crystal_density_diffrn    1.427
_exptl_crystal_description       block
_exptl_crystal_F_000             1236
_refine_diff_density_max         1.061
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         9784
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.073
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0694P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6320
_reflns_number_total             9784
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00536e2.cif
_cod_data_source_block           p
_cod_original_cell_volume        2778.5(19)
_cod_database_code               4349638
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N1 \\sim C56 \\sim C57: within 1.7A with sigma of 0.004 and sigma for terminal
atoms of 0.008
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B)
3.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C16(H16), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26),
  C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43), C44(H44),
  C45(H45), C46(H46), C47(H47), C48(H48), C51(H51), C52(H52), C53(H53),
 C54(H54), C55(H55)
3.c Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C58(H58A,H58B,H58C)
;
_olex2_submission_special_instructions 'No special instructions were received'