Systematic Investigation of Trigonal-Bipyramidal Cyanide-Bridged Clusters of the First-Row Transition Metals
Mikhail Shatruk; Kristen E. Chambers; Andrey V. Prosvirin; Kim R. Dunbar; Inorganic Chemistry 46 (2007) 5155–5165; doi:10.1021/ic061856t

data_4307310
_publ_contact_author_address
; 
Department of Chemistry
Texas A&M University
PO Box 30012 
College Station 
Texas 77842-3012 
USA
;
_publ_contact_author_email       dunbar@mail.chem.tamu.edu
_publ_contact_author_fax         (979)8457177
_publ_contact_author_name        'Dunbar, Kim R.'
_publ_contact_author_phone       (979)8625235
_publ_section_title
;
Systematic Investigation of Trigonal-Bipyramidal Cyanide-Bridged Clusters
of the First-Row Transition Metals
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5155
_journal_page_last               5165
_journal_paper_doi               10.1021/ic061856t
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C108 H96 Co2 N24 Ni3'
_chemical_formula_weight         2024.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 98.031(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.225(2)
_cell_length_b                   25.009(3)
_cell_length_c                   24.716(3)
_cell_measurement_reflns_used    543
_cell_measurement_temperature    150(2)
_cell_volume                     11767(2)
_computing_cell_refinement       'SMART V5.625 (Bruker, 2000)'
_computing_data_collection       'SMART V5.625 (Bruker, 2000)'
_computing_data_reduction        'SAINT V6.32 (Bruker, 2001)'
_computing_molecular_graphics    'X-Seed (Barbour, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.835
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'profile data from \w scans'
_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  0.0519
_diffrn_reflns_av_sigmaI/netI    0.1204
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            44637
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.8896
_exptl_absorpt_correction_T_min  0.6908
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4200
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.15
_platon_squeeze_details          ' ?'
_refine_diff_density_max         1.871
_refine_diff_density_min         -0.574
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1258
_refine_ls_number_reflns         24395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0678
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1473
_refine_ls_wR_factor_ref         0.1596
_reflns_number_gt                10444
_reflns_number_total             24395
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061856tsi20061216_075334.cif
_cod_data_source_block           c:\structures\mike\ms094\p21_c
_cod_database_code               4307310