31P NMR Studies Demonstrating the Assembly ofcatena-Phosphorus Frameworks from Chlorophosphinochlorophosphonium Cations
Yuen-ying Carpenter; Neil Burford; Michael, D. Lumsden; Robert McDonald; Inorganic Chemistry 50 (2011) 3342–3353; doi:10.1021/ic102150s

data_4324843
_publ_contact_author_address
; Department of Chemistry
  University of Alberta
  Edmonton, Alberta T6G 2G2
  Canada
;
_publ_contact_author_email       neil.burford@dal.ca
_publ_contact_author_fax         1(902)4941310
_publ_contact_author_name        'Dr Neil Burford'
_publ_contact_author_phone       1(902)4943707
_publ_section_title
;
 31P NMR Studies Demonstrating the Assembly ofcatena-Phosphorus Frameworks
 from Chlorophosphinochlorophosphonium Cations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3342
_journal_page_last               3353
_journal_paper_doi               10.1021/ic102150s
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C21 H49 P5, 2(Cl4 Ga), C H2 Cl2'
_chemical_formula_sum            'C22 H51 Cl10 Ga2 P5'
_chemical_formula_weight         964.42
_chemical_name_systematic
; 
 ? 
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.2769(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6226(11)
_cell_length_b                   22.014(2)
_cell_length_c                   16.9005(15)
_cell_measurement_reflns_used    9808
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      2.20
_cell_volume                     4279.1(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_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  0.0174
_diffrn_reflns_av_sigmaI/netI    0.0152
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            37146
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    2.086
_exptl_absorpt_correction_T_max  0.5373
_exptl_absorpt_correction_T_min  0.3750
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_description       prism
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.041
_refine_diff_density_min         -0.777
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         9779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0575P)^2^+4.4235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1136
_reflns_number_gt                8272
_reflns_number_total             9779
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic102150s_si_002.cif
_cod_data_source_block           12{iPr}-{GaCl4}2-CH2Cl2
_cod_original_cell_volume        4279.0(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4324843