Acidic Dicationic Iron(II) Dihydrogen Complexes and Compounds Related by H2 Substitution
Shaun E. Landau; Robert H. Morris; Alan J. Lough; Inorganic Chemistry 38 (1999) 6060–6068; doi:10.1021/ic990876a

data_4322576
_publ_section_title
;
 Acidic Dicationic Iron(II) Dihydrogen Complexes and Compounds Related by
 H2 Substitution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6060
_journal_page_last               6068
_journal_paper_doi               10.1021/ic990876a
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C21 H48 B2 F8 Fe O P4'
_chemical_formula_weight         669.95
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 96.23(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.270(2)
_cell_length_b                   15.014(3)
_cell_length_c                   39.908(8)
_cell_measurement_temperature    173.0(1)
_cell_volume                     6117(2)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'KappaCCD server software (Nonius, 1997)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL V5.1'
_computing_publication_material  'Bruker SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173.0(1)
_diffrn_measured_fraction_theta_full 0.654
_diffrn_measured_fraction_theta_max 0.654
_diffrn_measurement_device_type  'Nonius Kappa-CCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_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  0.054
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            26825
_diffrn_reflns_theta_full        24.04
_diffrn_reflns_theta_max         24.04
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo-SMN, (Otwinowski & Minor, 1997)'
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2800
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.546
_refine_diff_density_rms         0.080
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.57(2)
_refine_ls_extinction_coef       0.0031(3)
_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   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1330
_refine_ls_number_reflns         11920
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0608
_refine_ls_shift/su_max          0.177
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+24.9187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1560
_reflns_number_gt                10470
_reflns_number_total             11920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990876a_1.cif
_cod_data_source_block           k9806rv1_Complex7[BF4]
_cod_original_sg_symbol_H-M      'P 1 21/m 1'
_cod_database_code               4322576