Hexakis(μ~4~-2-amino-2-methylpropane-1,3-diolato)hexachloroheptairon(II,III) acetonitrile disolvate monohydrate
Gaël Labat; Colette Boscovic; Hans U. Güdel; Acta Crystallographica Section E 61 (2005) m611–m613; doi:10.1107/S160053680500557X

data_2205573
_publ_section_title
;Hexakis(\m~4~-2-amino-2-methylpropane-1,3-diolato)hexachloroheptairon(II,III)
 acetonitrile disolvate monohydrate
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m611
_journal_page_last               m613
_journal_paper_doi               10.1107/S160053680500557X
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '[Fe7 (C4 H9 N O2)6 Cl6] , 2C H3 C N , H2 O'
_chemical_formula_moiety         'C24 H54 Cl6 Fe7 N6 O12 , 2C2 H3 N , H2 O'
_chemical_formula_sum            'C28 H62 Cl6 Fe7 N8 O13'
_chemical_formula_weight         1322.51
_chemical_name_systematic
;
Hexakis(\m~4~-2-amino-2-methylpropane-1,3-diolato)hexachloroheptairon(II,III)
acetonitrile disolvate monohydrate
;
_space_group_IT_number           148
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.4150(7)
_cell_length_b                   12.4150(7)
_cell_length_c                   28.030(3)
_cell_measurement_reflns_used    3857
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      2.15
_cell_volume                     3741.5(5)
_computing_cell_refinement       'CELL in IPDS II'
_computing_data_collection       'EXPOSE in IPDS II (Stoe, 2000)'
_computing_data_reduction        'INTEGRATE in IPDS II (Stoe, 2000)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 0.81
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '\f oscillation'
_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  0.1797
_diffrn_reflns_av_sigmaI/netI    0.1320
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            9917
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         2.03
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.360
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS in PLATON; Spek, 2003)'
_exptl_crystal_colour            block
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       brown
_exptl_crystal_F_000             2022
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.519
_refine_diff_density_min         -1.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.883
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     105
_refine_ls_number_reflns         1622
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.1140
_refine_ls_R_factor_gt           0.0652
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0981P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1560
_refine_ls_wR_factor_ref         0.1688
_reflns_number_gt                916
_reflns_number_total             1622
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om6230.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2205573
_cod_database_fobs_code          2205573