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

data_7041730
_publ_section_title
;
 Syntheses of Transition Metal Methoxysiloxides
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C6DT04205H
_journal_year                    2017
_chemical_formula_moiety
; 
C30 H45 Cu N2 O3 Si, 0.5(C7 H8), 0.5(C4 H10 O) 
;
_chemical_formula_sum            'C35.5 H54 Cu N2 O3.5 Si'
_chemical_formula_weight         656.43
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2016-10-31 deposited with the CCDC.
2017-01-17 downloaded from the CCDC.
;
_cell_angle_alpha                107.402(4)
_cell_angle_beta                 94.625(4)
_cell_angle_gamma                113.436(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9765(7)
_cell_length_b                   12.7863(8)
_cell_length_c                   15.3713(10)
_cell_measurement_reflns_used    7110
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.69
_cell_measurement_theta_min      2.24
_cell_volume                     1839.0(2)
_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, TWINABS V2012/1 
(Bruker, 2012 & 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 0.990
_diffrn_measurement_device       '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  cm66qsa
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            36784
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.501
_diffrn_reflns_theta_min         2.086
_exptl_absorpt_coefficient_mu    0.662
_exptl_absorpt_correction_T_max  0.99968
_exptl_absorpt_correction_T_min  0.99896
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS V2014/4 (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             704
_exptl_crystal_id                cm66qsa
_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 3) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.823
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         6787
_refine_ls_number_restraints     587
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0556P)^2^+1.9419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5313
_reflns_number_total             6787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04205h2.cif
_cod_data_source_block           cm66qsa
_cod_original_formula_sum        'C35.50 H54 Cu N2 O3.50 Si'
_cod_database_code               7041730
_shelx_estimated_absorpt_t_min   0.839
_shelx_estimated_absorpt_t_max   0.951
_shelxl_version_number           2014/6
_shelx_res_checksum              50785