Phosphanyl-substituted π-excess σ2P heterocycles: Coordination behaviour of 2-di-tert-butylphosphanyl-1-neopentyl-1,3-benzazaphosphole towards CuCl, HgCl2 and [Rh(COD)2]BF4
Ghalib, Mohammed; Jones, Peter G.; Palm, Gottfried J.; Heinicke, Joachim W.; RSC Advances 3 (2013) 17726–; doi:10.1039/c3ra43706j

data_7239232
_publ_section_title
;
 Phosphanyl-substituted \p-excess \s2P heterocycles: Coordination
 behaviour of 2-di-tert-butylphosphanyl-1-neopentyl-1,3-benzazaphosphole
 towards CuCl, HgCl2 and [Rh(COD)2]BF4
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              17726
_journal_paper_doi               10.1039/c3ra43706j
_journal_volume                  3
_journal_year                    2013
_chemical_formula_sum            'C28 H46 B F3 N O P2 Rh'
_chemical_formula_weight         645.32
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.102(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.70896(15)
_cell_length_b                   18.3370(3)
_cell_length_c                   14.9610(2)
_cell_measurement_reflns_used    37610
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.2234
_cell_measurement_theta_min      2.1982
_cell_volume                     2937.35(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1419
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur, Eos'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0175
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            95434
_diffrn_reflns_theta_full        28.50
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1344
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.936
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     359
_refine_ls_number_reflns         7619
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+2.8771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0737
_refine_ls_wR_factor_ref         0.0780
_reflns_number_gt                6686
_reflns_number_total             7619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra43706j.txt
_cod_data_source_block           grobuu
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2937.36(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7239232