Solid-State 115In and 31P NMR Studies of Triarylphosphine Indium Trihalide Adducts
Fu Chen; Guibin Ma; Guy M. Bernard; Ronald G. Cavell; Robert McDonald; Michael J. Ferguson; Roderick E. Wasylishen; Journal of the American Chemical Society 132 (2010) 5479–5493; doi:10.1021/ja100625p

data_4102276
_publ_contact_author_address
; Department of Chemistry
  University of Alberta
  Edmonton, Alberta T6G 2G2
  Canada
;
_publ_contact_author_email       Roderick.Wasylishen@ualberta.ca
_publ_contact_author_fax         1(780)4928231
_publ_contact_author_name        'Dr. Roderick E. Wasylishen'
_publ_contact_author_phone       1(780)4924336
_publ_section_title
;
 Solid-State 115In and 31P NMR Studies of Triarylphosphine Indium
 Trihalide Adducts
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5479
_journal_page_last               5493
_journal_paper_doi               10.1021/ja100625p
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C21 H21 Br3 In O3 P'
_chemical_formula_sum            'C21 H21 Br3 In O3 P'
_chemical_formula_weight         706.90
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'manual editing of SHELXL template'
_cell_angle_alpha                90.00
_cell_angle_beta                 99.882(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.851(3)
_cell_length_b                   11.134(3)
_cell_length_c                   18.831(4)
_cell_measurement_reflns_used    5944
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.28
_cell_measurement_theta_min      2.20
_cell_volume                     2447.9(10)
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_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  0.0844
_diffrn_reflns_av_sigmaI/netI    0.0703
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18700
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.74
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.946
_exptl_absorpt_correction_T_max  0.4691
_exptl_absorpt_correction_T_min  0.1995
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.918
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.309
_refine_diff_density_min         -1.915
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         5013
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0991P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1637
_reflns_number_gt                3768
_reflns_number_total             5013
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja100625p_si_002.cif
_cod_data_source_block           Br3In[P(o-Anis)3](4)
_cod_original_cell_volume        2448.0(10)
_cod_database_code               4102276