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_4345463
_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
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 119.199(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.0932(9)
_cell_length_b                   18.0034(8)
_cell_length_c                   12.9943(9)
_cell_measurement_reflns_used    32568
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2673.8(4)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_molecular_graphics
; 
 'Rigaku R-AXIS RAPID, Rigaku R_AXIS RAPID imaging plate' 
;
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID imaging plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1079
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            60140
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.136
_diffrn_source                   'Sealed Tube'
_exptl_absorpt_coefficient_mu    0.628
_exptl_absorpt_correction_T_max  0.963
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private Communication'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         6112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0570
_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^)+(0.0475P)^2^+2.4236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4782
_reflns_number_total             6112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b01952_si_004.cif
_cod_data_source_block           spider-14137
_cod_original_cell_volume        2673.8(3)
_cod_database_code               4345463
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.963
_shelxl_version_number           2014/6
_shelx_res_checksum              52105
_shelx_hkl_checksum              9322