Double Silyl Migration Converting ORe[N(SiMe2CH2PCy2)2] to NRe[O(SiMe2CH2PCy2)2] Substructures
Oleg V. Ozerov; Hélène F. Gerard; Lori A. Watson; John C. Huffman; Kenneth G. Caulton; Inorganic Chemistry 41 (2002) 5615–5625; doi:10.1021/ic020424p

data_5000299
_publ_section_title
;
Double Silyl Migration Converting ORe[N(SiMe2CH2PCy2)2] to
NRe[O(SiMe2CH2PCy2)2] Substructures
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5615
_journal_page_last               5625
_journal_paper_doi               10.1021/ic020424p
_journal_volume                  41
_journal_year                    2002
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H60 Cl2 N O P2 Re Si2'
_chemical_formula_weight         826.043
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method
'minor manual editing of SDT2CIF v. 1.2 BETA  output'
_cell_angle_alpha                90
_cell_angle_beta                 100.6530
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2394(3)
_cell_length_b                   13.2263(3)
_cell_length_c                   24.2823(6)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    ?
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.40
_cell_volume                     3547.49(15)
_computing_data_reduction        'SAINT (Bruker, 1999), XTEL (local package)'
_diffrn_ambient_temperature      ?
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
'   0.30 degree frames measured for   5.17 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            96977
_diffrn_reflns_theta_full        29.9924
_diffrn_reflns_theta_max         29.9924
_diffrn_reflns_theta_min         2.16782
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_time  313
_diffrn_standards_number         9836
_exptl_absorpt_coefficient_mu    3.7606
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       multifaceted
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .18
_refine_diff_density_max         1.68
_refine_diff_density_min         -0.4
_refine_ls_abs_structure_details none
_refine_ls_abs_structure_Flack   ?
_refine_ls_extinction_coef       -0.000000045(6)
_refine_ls_extinction_expression
;
Larson, A. C. (1967).  Acta Cryst. 23, p. 664.  Eq. (3)
;
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_ref   0.4336
_refine_ls_hydrogen_treatment    ?
_refine_ls_matrix_type           full
_refine_ls_number_parameters     593
_refine_ls_number_reflns         7742
_refine_ls_R_factor_gt           0.0160
_refine_ls_shift/su_max          0.0549
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w^-1^=\s^2^(F)+(.07F)^2^
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0189
_reflns_number_gt                7742
_reflns_number_total             10364
_reflns_threshold_expression     'Fo^2^> 2.33\s(Fo^2^)'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C30 H60 Cl2 N1 O1 P2 Re1 Si2'
_cod_database_code               5000299