Cooperative Metal‒Ligand Reactivity and Catalysis in Low-Spin Ferrous Alkoxides
Chu, Wan-Yi; Zhou, Xiaoyuan; Rauchfuss, Thomas B.; Organometallics 34 (2015) 1619–; doi:10.1021/om501152h

data_4085461
_publ_section_title
;
 Cooperative Metal--Ligand Reactivity and Catalysis in Low-Spin Ferrous
 Alkoxides
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              1619
_journal_paper_doi               10.1021/om501152h
_journal_volume                  34
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C41 H33 Fe N O3 P2'
_chemical_formula_sum            'C41 H33 Fe N O3 P2'
_chemical_formula_weight         705.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-10-07
_audit_creation_method
; 
Olex2 1.2 
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874) 
;
_cell_angle_alpha                90
_cell_angle_beta                 111.171(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.505(3)
_cell_length_b                   16.422(4)
_cell_length_c                   10.768(3)
_cell_measurement_reflns_used    4234
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.89
_cell_measurement_theta_min      2.32
_cell_volume                     1732.2(8)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2013/3, SADABS V2012/1, TWINABS V2012/1 
(Bruker, 2012 & 2013) 
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173.15
_diffrn_detector                 'Bruker APEXII CCD area detector'
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa/ApexII CCD'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm63g_0m
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            19041
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.530
_diffrn_reflns_theta_min         2.028
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.9950
_exptl_absorpt_correction_T_min  0.8924
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.0902 before and 0.0555 after correction. 
The Ratio of minimum to maximum transmission is 0.8969. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       plate
_exptl_crystal_F_000             732
_exptl_crystal_id                cm63g_0m
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 -2 2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
; 
 Flack x determined using 2329 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.026(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         6324
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0345P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0795
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.965
_reflns_number_gt                5489
_reflns_number_total             6324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501152h_si_001.cif
_cod_data_source_block           Fe(P2O2)(CO)(NCMe)
_cod_depositor_comments
'Adding full bibliography for 4085461--4085465.cif.'
_cod_original_cell_volume        1732.2(7)
_cod_database_code               4085461
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.842
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Ternary CH refined with riding coordinates: 
 C4(H4), C5(H5) 
2.b Aromatic/amide H refined with riding coordinates: 
 C7(H7), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16), 
 C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), 
  C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35), 
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41) 
2.c Idealised Me refined as rotating group: 
 C3(H3A,H3B,H3C) 
;
_olex2_submission_special_instructions 'No special instructions were received'