A diketiminate-bound diiron complex with a bridging carbonate ligand
Sadique, Azwana R.; Brennessel, William W.; Holland, Patrick L.; Acta Crystallographica Section C 65 (2009) m174–m176; doi:10.1107/S0108270109011275

data_2017107
_publ_section_title
;
 A diketiminate-bound diiron complex with a bridging carbonate ligand
;
_journal_coeditor_code           MX3010
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m174
_journal_page_last               m176
_journal_paper_doi               10.1107/S0108270109011275
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Fe2 (C41 H65 N)2 (C O3)] , 2C7 H8'
_chemical_formula_moiety         'C83 H130 Fe2 N4 O3 , 2C7 H8'
_chemical_formula_sum            'C97 H146 Fe2 N4 O3'
_chemical_formula_weight         1527.88
_chemical_name_common            holas13
_chemical_name_systematic
;
\m-carbonato-\k^3^<i>O</i>:<i>O</i>',<i>O</i>''-
bis{[2,2,6,6-tetramethyl-3,5-bis(2,4,6-triisopropylphenyl)heptane-2,5-
diiminate(1-)-\k^2^<i>N</i>,<i>N</i>']iron(II)} toluene disolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                77.533(3)
_cell_angle_beta                 79.815(3)
_cell_angle_gamma                70.941(3)
_cell_formula_units_Z            2
_cell_length_a                   14.7703(7)
_cell_length_b                   15.5535(8)
_cell_length_c                   21.6991(11)
_cell_measurement_reflns_used    3016
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.32
_cell_volume                     4569.9(4)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008<i>b</i>)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008<i>b</i>)'
_diffrn_ambient_temperature      100.00(10)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
'Bruker SMART APEXII Platform CCD area-detector'
_diffrn_measurement_method       'area dectector, \w scans per \f'
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0444
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            71339
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.418
_refine_diff_density_min         -0.364
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1199
_refine_ls_number_reflns         26363
_refine_ls_number_restraints     275
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0420
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0464P)^2^+1.0611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                19303
_reflns_number_total             26363
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            mx3010.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2017107
_cod_database_fobs_code          2017107