10-(<i>tert</i>-Butyldimethylsilyl)-4,6-bis(diphenylphosphino)phenoxazine
Osiński, Piotr W.; Schürmann, Markus; Preut, Hans; Haag, Rainer; Eilbracht, Peter; Acta Crystallographica Section E 61 (2005) o3115–o3116; doi:10.1107/S1600536805027121

data_2206868
_publ_section_title
;
 10-(<i>tert</i>-Butyldimethylsilyl)-4,6-bis(diphenylphosphino)phenoxazine
;
_journal_coeditor_code           BT6724
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3115
_journal_page_last               o3116
_journal_paper_doi               10.1107/S1600536805027121
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C42 H41 N O P2 Si'
_chemical_formula_moiety         'C42 H41 N O P2 Si'
_chemical_formula_sum            'C42 H41 N O P2 Si'
_chemical_formula_weight         665.79
_chemical_name_systematic
;
10-(tert-Butyldimethylsilyl)-4,6-bis(diphenylphosphino)phenoxazine
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.139(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.8748(18)
_cell_length_b                   10.8973(10)
_cell_length_c                   19.1042(15)
_cell_measurement_reflns_used    32114
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      3.2
_cell_volume                     3712.2(6)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'DENZO and SCALEPACK'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1991)'
_computing_publication_material
;
SHELXL97, PARST95 (Nardelli, 1995) and PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_sigmaI/netI    0.1730
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            32114
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.20
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.182
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.1542
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = [exp{4.2(sin\q/\l)^2^}]/[\s^2^(Fo^2^)] where P = 0.333Fo^2^ + 0.667Fc^2^'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0619
_refine_ls_wR_factor_ref         0.0793
_reflns_number_gt                2229
_reflns_number_total             6468
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6724.cif
_cod_data_source_block           I
_cod_original_sg_symbol_Hall     '-p 2yn'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2206868
_cod_database_fobs_code          2206868