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_4085463
_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            'C43 H38 Cl2 F6 Fe O12 P2 S2'
_chemical_formula_weight         1113.54
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 90.340(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   43.471(3)
_cell_length_b                   11.9162(6)
_cell_length_c                   17.6349(11)
_cell_measurement_reflns_used    9892
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.31
_cell_volume                     9134.9(10)
_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
; 
? 
;
_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      102(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd31msa_sq
_diffrn_reflns_av_R_equivalents  0.0573
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44247
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.385
_diffrn_reflns_theta_min         2.213
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.696
_exptl_absorpt_correction_T_max  0.99972
_exptl_absorpt_correction_T_min  0.99916
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SHELXTL/XPREP V2013/3 (Bruker, 2013)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_description       plate
_exptl_crystal_F_000             4544
_exptl_crystal_id                cd31msa_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 (-2 3 -1) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.05
_platon_squeeze_details
; 
The disordered model suggest that there were 2 additional water molecules in the 
asymmetric unit. This accounts for 16 additional water molecules in the unit 
cell. The number of electrons "squeezed" from the model is consistent with 
that predicted from the disordered model. 
 
TITL cd31msa in C2/c 
CELL   43.4710   11.9162   17.6349     90.00     90.34     90.00 
SPGR C2/c 
C101 0.993 0.219 0.816 !      14.80 eA-3 
C102 0.511 0.480 0.219 !      12.67 eA-3 
C103 1.000 0.219 0.749 !       1.99 eA-3 
Q104 0.508 0.353 0.873 !       0.84 eA-3 
Q105 0.137 0.374 0.484 !       0.83 eA-3 
Q106 0.642 0.326 0.842 !       0.83 eA-3 
C107 1.000 0.109 0.748 !       0.82 eA-3 
C108 0.485 0.441 0.201 !       0.82 eA-3 
Q109 0.243 0.258 0.497 !       0.81 eA-3 
Q110 0.738 0.175-0.001 !       0.81 eA-3 
Q111 0.747 0.350 0.968 !       0.78 eA-3 
Q112 0.187 0.466 0.248 !       0.75 eA-3 
Q113 0.735 0.381 0.637 !       0.74 eA-3 
Q114 0.176 0.100 0.653 !       0.70 eA-3 
Q115 0.806 0.101 0.464 !       0.69 eA-3 
Q116 0.585 0.017 0.809 !       0.69 eA-3 
Q117 0.430 0.213 0.737 !       0.68 eA-3 
Q118 0.700 0.346 0.826 !       0.67 eA-3 
Q119 0.078 0.065 0.140 !       0.66 eA-3 
Q120 0.804 0.071 0.699 !       0.66 eA-3 
Q121 0.871 0.230 0.176 !       0.66 eA-3 
Q122 0.875 0.376 0.112 !       0.65 eA-3 
Q123 0.533 0.438 0.200 !       0.64 eA-3 
Q124 0.101 0.431 0.489 !       0.64 eA-3 
Q125 0.956 0.473 0.265 !       0.64 eA-3 
Q126 0.157 0.490 0.347 !       0.64 eA-3 
Q127 0.672 0.075 0.781 !       0.62 eA-3 
Q128 0.860 0.371 0.161 !       0.61 eA-3 
Q129 0.533 0.502 0.705 !       0.60 eA-3 
Q130 0.195 0.429 0.807 !       0.60 eA-3 
Q131 1.000 0.235 0.342 !       0.60 eA-3 
Q132 0.874 0.302 0.147 !       0.60 eA-3 
Q133 0.077 0.052 0.097 !       0.60 eA-3 
Q134 0.242 0.478 0.984 !       0.59 eA-3 
Q135 0.414 0.300 0.759 !       0.59 eA-3 
Q136 0.617 0.457 0.295 !       0.59 eA-3 
Q137 0.327 0.419 0.221 !       0.59 eA-3 
Q138 0.817 0.354 0.434 !       0.59 eA-3 
Q139 0.871 0.052 0.203 !       0.59 eA-3 
C140 0.512 0.505 0.657 !       0.59 eA-3 
Q141 0.429 0.303 0.645 !       0.58 eA-3 
Q142 0.415 0.379 0.382 !       0.58 eA-3 
Q143 0.104 0.446 0.567 !       0.58 eA-3 
Q144 0.719 0.321 0.670 !       0.58 eA-3 
Q145 0.332 0.318 0.920 !       0.57 eA-3 
Q146 0.284 0.393 0.251 !       0.57 eA-3 
Q147 0.937 0.141 0.580 !       0.56 eA-3 
Q148 0.618 0.118 0.920 !       0.55 eA-3 
Q149 0.989 0.293 0.989 !       0.55 eA-3 
Q150 0.827 0.497 0.264 !       0.55 eA-3 
C151 0.988 0.153 0.700 !       0.54 eA-3 
Q152 0.891 0.348 0.178 !       0.54 eA-3 
Q153 0.961 0.372 0.271 !       0.54 eA-3 
Q154 0.164 0.455 0.888 !       0.54 eA-3 
Q155 0.984 0.079 0.276 !       0.54 eA-3 
Q156 0.558 0.117 0.784 !       0.54 eA-3 
Q157 0.608 0.501 0.184 !       0.53 eA-3 
Q158 0.515 0.368 0.136 !       0.53 eA-3 
Q159 0.618 0.295 0.845 !       0.53 eA-3 
Q160 0.125 0.212 0.855 !       0.53 eA-3 
Q161 0.504 0.167 0.190 !       0.52 eA-3 
Q162 0.723 0.344 0.204 !       0.52 eA-3 
Q163 0.581 0.124 0.776 !       0.52 eA-3 
Q164 0.140 0.068 0.500 !       0.51 eA-3 
Q165 0.673 0.315 0.641 !       0.51 eA-3 
Q166 0.558 0.301 0.921 !       0.51 eA-3 
Q167 0.644 0.332 0.653 !       0.51 eA-3 
Q168 0.371 0.452 0.202 !       0.51 eA-3 
Q169 0.125 0.188 0.238 !       0.51 eA-3 
Q170 0.703 0.291 0.595 !       0.51 eA-3 
Q171 0.137 0.142 0.299 !       0.51 eA-3 
Q172 0.527 0.135 0.032 !       0.50 eA-3 
Q173 0.294 0.038 0.451 !       0.50 eA-3 
;
_refine_diff_density_max         0.793
_refine_diff_density_min         -1.288
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         8406
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0726P)^2^+55.2882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1358
_refine_ls_wR_factor_ref         0.1456
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6773
_reflns_number_total             8406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om501152h_si_001.cif
_cod_data_source_block           Fe[P2(OH)2](CO)2(OTf)2
_cod_depositor_comments
'Adding full bibliography for 4085461--4085465.cif.'
_cod_original_cell_volume        9134.9(9)
_cod_database_code               4085463
_shelx_estimated_absorpt_t_min   0.890
_shelx_estimated_absorpt_t_max   0.966
_shelxl_version_number           2014-3
_shelx_res_checksum              11083
_shelx_hkl_checksum              73832
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              8777