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_4085462
_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_formula_moiety         'C42 H39 Fe O3 P3, 2(C H2 Cl2)'
_chemical_formula_sum            'C44 H43 Cl4 Fe O3 P3'
_chemical_formula_weight         910.34
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-09-05
_audit_creation_method
; 
Olex2 1.2 
(compiled 2014.08.28 svn.r2986 for OlexSys, GUI svn.r4874) 
;
_cell_angle_alpha                90
_cell_angle_beta                 95.781(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.342(2)
_cell_length_b                   19.477(4)
_cell_length_c                   21.417(5)
_cell_measurement_reflns_used    4350
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      23.72
_cell_measurement_theta_min      2.28
_cell_volume                     4292.1(16)
_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 0.998
_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  cm11h2_0m
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33747
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.383
_diffrn_reflns_theta_min         1.911
_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    0.751
_exptl_absorpt_correction_T_max  0.9779
_exptl_absorpt_correction_T_min  0.8422
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
; 
SADABS-2012/1 (Bruker,2012) was used for absorption correction. 
wR2(int) was 0.1046 before and 0.0553 after correction. 
The Ratio of minimum to maximum transmission is 0.8612. 
The \l/2 correction factor is 0.0015. 
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       column
_exptl_crystal_F_000             1880
_exptl_crystal_id                cm11h2_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 -1 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.398
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     499
_refine_ls_number_reflns         7872
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+1.6523P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.1096
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5320
_reflns_number_total             7872
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501152h_si_001.cif
_cod_data_source_block           Fe(P2O2)(CO)(PMe3)
_cod_depositor_comments
'Adding full bibliography for 4085461--4085465.cif.'
_cod_database_code               4085462
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.965
_shelx_estimated_absorpt_t_min   0.754
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2.a Ternary CH refined with riding coordinates: 
 C5(H5), C6(H6) 
2.b Secondary CH2 refined with riding coordinates: 
 C44(H44A,H44B), C43(H43A,H43B) 
2.c Aromatic/amide H refined with riding coordinates: 
 C8(H8), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), 
 C18(H18), C20(H20), C21(H21), C22(H22), C23(H23), C24(H24), 
  C26(H26), C27(H27), 
  C28(H28), C29(H29), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36), 
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42) 
2.d Idealised Me refined as rotating group: 
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C) 
;
_olex2_submission_special_instructions 'No special instructions were received'