Diazoalkanes in Low-Coordinate Iron Chemistry: Bimetallic Diazoalkyl and Alkylidene Complexes of Iron(II).
Reesbeck, Megan E.; Grubel, Katarzyna; Kim, Daniel; Brennessel, William W.; Mercado, Brandon Q.; Holland, Patrick L.; Inorganic chemistry 56 (2017) 1019–1022; doi:10.1021/acs.inorgchem.6b01952

data_4345466
_publ_section_title
;
 Diazoalkanes in Low-Coordinate Iron Chemistry: Bimetallic Diazoalkyl and
 Alkylidene Complexes of Iron(II).
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1019
_journal_page_last               1022
_journal_paper_doi               10.1021/acs.inorgchem.6b01952
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C52 H72 Fe2 N8 Si2'
_chemical_formula_sum            'C52 H72 Fe2 N8 Si2'
_chemical_formula_weight         977.05
_chemical_name_common            holkg30
_chemical_name_systematic
; 
 ? 
;
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
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_cell_angle_beta                 66.460(3)
_cell_angle_gamma                64.951(3)
_cell_formula_units_Z            1
_cell_length_a                   11.2308(17)
_cell_length_b                   11.5081(17)
_cell_length_c                   12.0683(18)
_cell_measurement_reflns_used    2167
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      22.57
_cell_measurement_theta_min      2.29
_cell_volume                     1272.4(3)
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_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1757
_diffrn_reflns_av_unetI/netI     0.1372
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
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_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            28537
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.030
_diffrn_reflns_theta_max         25.017
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_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_min  0.6382
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_exptl_crystal_colour            orange
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_exptl_crystal_description       needle
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_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
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_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0707
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+0.6981P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                2902
_reflns_number_total             4483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01952_si_005.cif
_cod_data_source_block           holkg30
_cod_database_code               4345466
_shelx_estimated_absorpt_t_min   0.858
_shelx_estimated_absorpt_t_max   0.949
_shelxl_version_number           2012-8
_shelx_res_checksum              35602
_shelx_hkl_checksum              67549