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_4085464
_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_sum            'C44 H42 Fe N2 O4 P2 S'
_chemical_formula_weight         812.64
_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   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 110.410(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2468(9)
_cell_length_b                   23.9190(14)
_cell_length_c                   15.9804(10)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.87
_cell_measurement_theta_min      2.37
_cell_volume                     5103.8(6)
_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_publication_material  'XCIF V2013-1 (Bruker, 2013)'
_computing_structure_refinement  'SHELX-2013-4 (Sheldrick, 2013)'
_computing_structure_solution    'SHELX-2013-4 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cm02f_0m_sq
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            81992
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.165
_diffrn_reflns_theta_min         1.604
_exptl_absorpt_coefficient_mu    0.434
_exptl_absorpt_correction_T_max  0.9473
_exptl_absorpt_correction_T_min  0.8132
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.058
_exptl_crystal_description       block
_exptl_crystal_F_000             1696
_exptl_crystal_id                cm02f_0m_sq
_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 1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.666
_exptl_crystal_size_mid          0.347
_exptl_crystal_size_min          0.186
_platon_squeeze_details
; 
The highly disordered model suggest that there are 3 additional tetrahydrofuran 
molecules in the asymmetric unit.  One of the solvate molecules is approximately 
half occupied.  This accounts for 10 additional THF molecules in the unit cell. 
The number of electrons "squeezed" from the model is consistant with that predic 
from the highly disordered model. 
TITL cm02f_0m in P21/n #14 
CELL   14.2468   23.9190   15.9804     90.00    110.41     90.00 
SPGR P21/n 
C101 0.094 0.884 0.889 !       5.52 eA-3 
C102 0.184 0.867 0.920 !       4.16 eA-3 
C103 0.401 0.298 0.669 !       4.04 eA-3 
C104 0.688 0.692 0.403 !       3.89 eA-3 
C105 0.970 0.156 0.156 !       3.80 eA-3 
C106 0.332 0.976 0.703 !       3.56 eA-3 
C107 0.660 0.527 0.108 !       2.84 eA-3 
C108 0.713 0.058 0.248 !       2.84 eA-3 
C109 0.810 0.081 0.307 !       2.68 eA-3 
C110 0.437 0.906 0.155 !       2.55 eA-3 
C111 0.032 0.588 0.639 !       2.35 eA-3 
C112 0.025 0.559 0.574 !       2.34 eA-3 
C113 0.263 0.984 0.626 !       2.32 eA-3 
C114 1.000 0.500 0.500 !       2.08 eA-3 
C115 0.439 0.945 0.027 !       2.04 eA-3 
C116 0.123 0.404 0.438 !       1.53 eA-3 
Q117 0.047 0.712 0.136 !       0.52 eA-3 
 
;
_refine_diff_density_max         0.314
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         11288
_refine_ls_number_restraints     242
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0370P)^2^+2.9326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0891
_refine_ls_wR_factor_ref         0.0959
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9026
_reflns_number_total             11288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501152h_si_001.cif
_cod_data_source_block           Fe[P2(OH)2](CO)(thiourea)
_cod_depositor_comments
'Adding full bibliography for 4085461--4085465.cif.'
_cod_database_code               4085464
_shelx_estimated_absorpt_t_min   0.761
_shelx_estimated_absorpt_t_max   0.924
_shelxl_version_number           2014-3
_shelx_res_checksum              66867
_shelx_hkl_checksum              22249
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              45275