Electronic Structure and Bonding in Iron(II) and Iron(I) Complexes Bearing Bisphosphine Ligands of Relevance to Iron-Catalyzed C-C Cross-Coupling.
Kneebone, Jared L.; Fleischauer, Valerie E.; Daifuku, Stephanie L.; Shaps, Ari A.; Bailey, Joseph M.; Iannuzzi, Theresa E.; Neidig, Michael L.; Inorganic chemistry 55 (2015) 272–; doi:10.1021/acs.inorgchem.5b02263

data_4344782
_publ_section_title
;
 Electronic Structure and Bonding in Iron(II) and Iron(I) Complexes
 Bearing Bisphosphine Ligands of Relevance to Iron-Catalyzed C-C
 Cross-Coupling.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              272
_journal_paper_doi               10.1021/acs.inorgchem.5b02263
_journal_volume                  55
_journal_year                    2015
_chemical_formula_moiety         'C124 H176 Br2 Fe2 P4, C4 H10 O'
_chemical_formula_sum            'C128 H186 Br2 Fe2 O P4'
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_chemical_name_common            neijk39
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 103.2648(14)
_cell_angle_gamma                90
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_cell_length_b                   14.2424(11)
_cell_length_c                   30.373(2)
_cell_measurement_reflns_used    4010
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      2.51
_cell_volume                     6145.2(8)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
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_computing_structure_solution    'SIR2011 (Burla et al., 2012)'
_diffrn_ambient_temperature      100.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
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_diffrn_reflns_limit_k_min       -17
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_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            74990
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.373
_diffrn_reflns_theta_max         26.409
_diffrn_reflns_theta_min         1.986
_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6548
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_exptl_absorpt_process_details   'SADABS (Sheldrick, 2014)'
_exptl_crystal_colour            'dark orange'
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_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         12610
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+6.0212P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0932
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_reflns_Friedel_coverage         0.000
_reflns_number_gt                7743
_reflns_number_total             12610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02263_si_002.cif
_cod_data_source_block           neijk39
_cod_original_cell_volume        6145.1(8)
_cod_database_code               4344782
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.827
_shelx_estimated_absorpt_t_max   0.875
_shelx_res_checksum              82469
_shelx_hkl_checksum              86831