Control of S-Based Aggregation: Designed Synthesis of NiM2 and Ni2M Trinuclear Complexes
Stephen P. Jeffery; Michael L. Singleton; Joseph H. Reibenspies; Marcetta Y. Darensbourg; Inorganic Chemistry 46 (2007) 179–185; doi:10.1021/ic061475f

data_4306993
_publ_contact_author_address
;Texas A&M University
Department of Chemistry
College Station, TX 77843-3255
USA            
;
_publ_contact_author_email       marcetta@mail.chem.tamu.edu
_publ_contact_author_fax         979-845-0158
_publ_contact_author_name        'Marcetta Y. Darensbourg'
_publ_contact_author_phone       959-845-5417
_publ_section_title
;
Control of S-Based Aggregation: Designed Synthesis of NiM2 and Ni2M
Trinuclear Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              179
_journal_page_last               185
_journal_paper_doi               10.1021/ic061475f
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C20 H40 Br Cu N4 Ni2 O4 S4'
_chemical_formula_weight         789.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.467(5)
_cell_length_b                   11.600(7)
_cell_length_c                   27.870(16)
_cell_measurement_temperature    110(2)
_cell_volume                     2737(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.887
_diffrn_measured_fraction_theta_max 0.887
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.1623
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            5271
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    3.932
_exptl_crystal_density_diffrn    1.916
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1616
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.824
_refine_diff_density_rms         0.161
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         3685
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1353
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                2217
_reflns_number_total             3685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061475fsi20060804_042402_1.cif
_cod_data_source_block           mdsj01
_cod_depositor_comments
;

2020-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         394.84
_cod_original_formula_units_Z            8
_cod_original_formula_sum        'C10 H20 Br0.50 Cu0.50 N2 Ni O2 S2'
_cod_database_code               4306993