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_4349637
_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 Cu Ni P4 S2, B F4, 2(C Cl2)'
_chemical_formula_sum            'C57 H80 B Cl4 Cu F4 Ni P4 S2'
_chemical_formula_weight         1304.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_audit_creation_date             2016-05-23
_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                85.6233(12)
_cell_angle_beta                 88.5791(15)
_cell_angle_gamma                87.8205(13)
_cell_formula_units_Z            4
_cell_length_a                   11.6179(3)
_cell_length_b                   19.8499(4)
_cell_length_c                   26.7528(5)
_cell_measurement_reflns_used    8110
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.599
_cell_measurement_theta_min      2.546
_cell_volume                     6145.6(2)
_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 0.973
_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  0.0615
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            56892
_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         25.000
_diffrn_reflns_theta_min         2.544
_exptl_absorpt_coefficient_mu    1.047
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       solid
_exptl_crystal_F_000             2720
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.259
_refine_diff_density_min         -0.721
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1369
_refine_ls_number_reflns         21602
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1056
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1068P)^2^+18.5780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.2034
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14587
_reflns_number_total             21602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00536e2.cif
_cod_data_source_block           p
_cod_database_code               4349637
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.930
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
F1 \\sim F1AA \\sim F4 \\sim F6 \\sim F14 \\sim F16 \\sim F26 \\sim B242:
within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
F1 \\sim F4 \\sim F6 \\sim F14 \\sim F16 \\sim F26 \\sim B242: within 1.7A with
sigma of 0.002 and sigma for terminal atoms of 0.004
F1 \\sim F4 \\sim F6 \\sim F14 \\sim F16 \\sim F26: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
2. Others
 Fixed Sof: C1AA(0.5) C109(0.5) F1(0.5) F4(0.5) F6(0.5) F14(0.5) F16(0.4)
 F26(0.6)
;
_shelx_res_checksum              69563
_shelx_hkl_checksum              82456
_olex2_submission_special_instructions 'No special instructions were received'