Probing Donor‒Acceptor Interactions inperi-Substituted Diphenylphosphinoacenaphthyl‒Element Dichlorides of Group 13 and 15 Elements
Hupf, Emanuel; Lork, Enno; Mebs, Stefan; Chęcińska, Lilianna; Beckmann, Jens; Organometallics 33 (2014) 7247–; doi:10.1021/om501036c

data_4084978
_publ_section_title
;
 Probing Donor--Acceptor Interactions inperi-Substituted
 Diphenylphosphinoacenaphthyl--Element Dichlorides of Group 13 and 15
 Elements
;
_journal_issue                   24
_journal_name_full               Organometallics
_journal_page_first              7247
_journal_paper_doi               10.1021/om501036c
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C24 H18 Cl2 Ga P'
_chemical_formula_weight         477.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.31(2)
_cell_angle_beta                 97.45(2)
_cell_angle_gamma                111.18(2)
_cell_formula_units_Z            2
_cell_length_a                   8.585(2)
_cell_length_b                   9.585(2)
_cell_length_c                   14.360(3)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.818
_cell_measurement_theta_min      5.494
_cell_volume                     1064.3(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens XSCANS'
_computing_molecular_graphics    Diamond
_computing_publication_material  WinGX
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '2\q/\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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0732
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3711
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.71
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.626
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6449
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
'Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             484
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3711
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0502
_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^)+(0.0696P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                2807
_reflns_number_total             3711
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501036c_si_003.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4084974--4084984.cif.'
_cod_original_cell_volume        1064.3(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084978