Di-μ-tricyanido-tetracyanidobis[hydrotris(pyrazoylborato)]tetramethanoldiiron(III)iron(II) dimethanol disolvate
Zhang, Kuirun; Sato, Osamu; Acta Crystallographica Section E 70 (2014) m56–; doi:10.1107/S1600536814001019

data_2238970
_publ_section_title
;
 Di-\m-tricyanido-tetracyanidobis[hydrotris(pyrazoylborato)]tetramethanoldiiron(III)iron(II)
 dimethanol disolvate
;
_journal_coeditor_code           PK2510
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m56
_journal_paper_doi               10.1107/S1600536814001019
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Fe3 (C9 H10 B N6)2 (C N)6 (C H4 O)4], 2C H4 O'
_chemical_formula_moiety         'C28 H36 B2 Fe3 N18 O4, 2(C1 H4 O1)'
_chemical_formula_sum            'C30 H44 B2 Fe3 N18 O6'
_chemical_formula_weight         942.00
_chemical_name_systematic
;Di-\m-tricyanido-tetracyanidobis[hydrotris(pyrazoylborato)]tetramethanoldiiron(III)iron(II)
dimethanol disolvate
;
_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                 94.671(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.261(4)
_cell_length_b                   16.405(7)
_cell_length_c                   14.331(6)
_cell_measurement_reflns_used    4554
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.11
_cell_volume                     2170.0(16)
_computing_cell_refinement       'CrystalClear (Rigaku, 2008)'
_computing_data_collection       'CrystalClear (Rigaku, 2008)'
_computing_data_reduction        'CrystalClear (Rigaku, 2008)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 7.314
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku Saturn70'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0965
_diffrn_reflns_av_sigmaI/netI    0.0704
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16575
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.11
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.051
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.946
_refine_diff_density_min         -0.815
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.132
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0638
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+4.4189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1670
_reflns_number_gt                4557
_reflns_number_total             4922
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            pk2510sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        2169.9(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2238970
_cod_database_fobs_code          2238970