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_4307315
_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            'C119 H96 Fe2 Mn3 N29.5 O2.5'
_chemical_formula_weight         2255.77
_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                 99.11(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.57(3)
_cell_length_b                   25.36(4)
_cell_length_c                   24.57(3)
_cell_measurement_reflns_used    201
_cell_measurement_temperature    120(2)
_cell_volume                     12040(3)
_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      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1500
_diffrn_reflns_av_sigmaI/netI    0.1656
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            96698
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.05
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.9591
_exptl_absorpt_correction_T_min  0.7609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03 (Bruker, 2003)'
_exptl_crystal_colour            brown-yellow
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4654
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.219
_refine_ls_extinction_coef       0.0049(4)
_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   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1383
_refine_ls_number_reflns         24596
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.2195
_refine_ls_R_factor_gt           0.0993
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1822P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2520
_refine_ls_wR_factor_ref         0.3313
_reflns_number_gt                10494
_reflns_number_total             24596
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061856tsi20061216_075503.cif
_cod_data_source_block           g:\michael\ms068\p21_c
_cod_original_cell_volume        12042(29)
_cod_original_formula_sum        'C119 H96 Fe2 Mn3 N29.50 O2.50'
_cod_database_code               4307315