Syntheses of Transition Metal Methoxysiloxides
Richers, Casseday P.; Bertke, Jeffery A.; Rauchfuss, Thomas; Dalton Trans.  (2017) –; doi:10.1039/C6DT04205H

data_7041732
_publ_section_title
;
 Syntheses of Transition Metal Methoxysiloxides
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C6DT04205H
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H48 Co O3 P3 Si, 0.5(C5 H12)'
_chemical_formula_sum            'C46.5 H54 Co O3 P3 Si'
_chemical_formula_weight         840.82
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-10-31 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9606(7)
_cell_length_b                   19.4711(13)
_cell_length_c                   21.7517(15)
_cell_measurement_reflns_used    9630
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.32
_cell_measurement_theta_min      2.33
_cell_volume                     4642.1(5)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
;
SAINT V8.34A, XPREP v2014/2, SADABS V2014/4 (Bruker, 2014) 
;
_computing_molecular_graphics
;
SHELXTL v2014-4 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       '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 tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0336
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            57504
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.437
_diffrn_reflns_theta_min         2.329
_exptl_absorpt_coefficient_mu    0.536
_exptl_absorpt_correction_T_max  0.94071
_exptl_absorpt_correction_T_min  0.85117
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1772
_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 3 -5) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.476
_exptl_crystal_size_mid          0.366
_exptl_crystal_size_min          0.256
_refine_diff_density_max         0.548
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details
;
 Flack x determined using 3675 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.004(6)
_refine_ls_extinction_coef       0.0107(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     634
_refine_ls_number_reflns         8493
_refine_ls_number_restraints     835
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0517
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0512P)^2^+7.9988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1296
_reflns_Friedel_coverage         0.936
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                8191
_reflns_number_total             8493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04205h2.cif
_cod_data_source_block           cd32ssaq
_cod_original_formula_sum        'C46.50 H54 Co O3 P3 Si'
_cod_database_code               7041732
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.785
_shelx_estimated_absorpt_t_max   0.875
_shelx_res_checksum              64312
_shelx_fab_checksum              55306