Proton-controlled formation and interconversion of AuI2NiII trinuclear and AuI4NiII3 heptanuclear complexes with mixed thiomalate and bis(diphenylphosphino)ethane
Kosuke Igawa; Nobuto Yoshinari; Takumi Konno; Chem.Commun. 50 (2014) 15573–; doi:10.1039/C4cc07578A

data_7116075
_publ_section_title
;
 Proton-controlled formation and interconversion of AuI2NiII trinuclear
 and AuI4NiII3 heptanuclear complexes with mixed thiomalate and
 bis(diphenylphosphino)ethane
;
_journal_name_full               Chem.Commun.
_journal_page_first              15573
_journal_paper_doi               10.1039/C4cc07578A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C37.5 H30.51 Au2 Na2 Ni O12 P2 S2'
_chemical_formula_sum            'C37.5 H30.51 Au2 Na2 Ni O12 P2 S2'
_chemical_formula_weight         1297.80
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 106.314(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.848(3)
_cell_length_b                   21.586(3)
_cell_length_c                   33.891(3)
_cell_measurement_reflns_used    7106
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.02
_cell_volume                     12531(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        PROCESS-AUTO
_computing_molecular_graphics    'CrystalStructure 4.1'
_computing_publication_material  'CrystalStructure 4.1 (Rigaku, 2014)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS2013 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS VII'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1232
_diffrn_reflns_av_unetI/netI     0.1357
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            92281
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.486
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'Rotating anode X-ray tube'
_diffrn_source_type              'Rigaku FR-E+ SuperBright'
_exptl_absorpt_coefficient_mu    5.141
_exptl_absorpt_correction_T_max  0.598
_exptl_absorpt_correction_T_min  0.162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Rigaku, 2014'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       block
_exptl_crystal_F_000             4972
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         7.194
_refine_diff_density_min         -4.403
_refine_diff_density_rms         0.424
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.822
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         28575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.822
_refine_ls_R_factor_all          0.2113
_refine_ls_R_factor_gt           0.1771
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5102
_refine_ls_wR_factor_ref         0.5240
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18514
_reflns_number_total             28575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc07578a3.cif
_cod_data_source_block           Na2[2]
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi-scans' was replaced
with the value 'multi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 

2024-03-12
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C75 H61 Au4 Na4 Ni2 O24 P4 S4'
_cod_original_formula_weight         2595.60
_cod_original_formula_moiety         'C75 H61 Au4 Na4 Ni2 O24 P4 S4'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        12532(3)
_cod_database_code               7116075
_shelx_estimated_absorpt_t_min   0.577
_shelx_estimated_absorpt_t_max   0.783
_shelxl_version_number           2014-3
_shelx_res_checksum              94144