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_4306994
_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 H20 N2 Ni O10 S2 W2'
_chemical_formula_weight         938.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                106.304(5)
_cell_angle_beta                 96.606(4)
_cell_angle_gamma                112.242(4)
_cell_formula_units_Z            2
_cell_length_a                   10.4829(7)
_cell_length_b                   10.5887(7)
_cell_length_c                   13.7992(8)
_cell_measurement_reflns_used    1950
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      57.38
_cell_measurement_theta_min      4.71
_cell_volume                     1317.83(16)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'MWPC area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0930
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11485
_diffrn_reflns_theta_full        58.93
_diffrn_reflns_theta_max         58.93
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    18.591
_exptl_absorpt_correction_T_max  0.8359
_exptl_absorpt_correction_T_min  0.0946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.366
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.060
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.00020(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         3652
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [0.00000+1.00000exp(1.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0000P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                2842
_reflns_number_total             3652
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061475fsi20060804_042402_2.cif
_cod_data_source_block           md307a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

2020-10-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H40 N4 Ni2 O20 S4 W4'
_cod_original_formula_weight         1877.82
_cod_original_formula_units_Z            1
_cod_original_cell_volume        1317.83(15)
_cod_database_code               4306994