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_4349639
_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         'C59 H54 Cu Ni P4 S2, B F4'
_chemical_formula_sum            'C59 H54 B Cu F4 Ni P4 S2'
_chemical_formula_weight         1160.08
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_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                87.551(3)
_cell_angle_beta                 77.012(3)
_cell_angle_gamma                83.794(3)
_cell_formula_units_Z            2
_cell_length_a                   11.637(4)
_cell_length_b                   14.059(5)
_cell_length_c                   19.665(7)
_cell_measurement_reflns_used    1882
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.555
_cell_measurement_theta_min      2.252
_cell_volume                     3116.0(19)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71000
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_av_unetI/netI     0.1644
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36636
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.859
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.9503
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       solid
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.678
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         10763
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.687
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0631
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1666P)^2^+0.2640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1637
_refine_ls_wR_factor_ref         0.2039
_reflns_number_gt                5175
_reflns_number_total             10763
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6qi00536e2.cif
_cod_data_source_block           p
_cod_original_cell_volume        3116.1(18)
_cod_database_code               4349639
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 B1-F1
 1.31 with sigma of 0.01
 B1-F4
 1.31 with sigma of 0.01
 B1-F3
 1.31 with sigma of 0.01
 B1-F2
 1.31 with sigma of 0.01
 F1-F4
 2.2 with sigma of 0.01
 F1-F3
 2.2 with sigma of 0.01
 F3-F4
 2.2 with sigma of 0.01
 F2-F4
 2.2 with sigma of 0.01
 F2-F1
 2.2 with sigma of 0.01
 F2-F3
 2.2 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
B1 \\sim F1 \\sim F2 \\sim F3 \\sim F4: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.002
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C46(H46A,H46B), C47(H47A,H47B)
4.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C41(H41), C42(H42),
  C43(H43), C44(H44), C45(H45), C49(H49), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54), C56(H56), C57(H57), C58(H58), C59(H59)
;
_olex2_submission_special_instructions 'No special instructions were received'