The change in the X-ray dipole moment as a quantitative measure of the polarizing effect of the molecular environment: application to a complex of p-amino-p′-nitrobiphenyl with triphenylphosphine oxide
Zhang, Yuegang; Coppens, Philip; Chemical Communications  (1999) 2425–; doi:10.1039/a907473b

data_7110718
_publ_section_title
;
 The change in the X-ray dipole moment as a quantitative measure of the
 polarizing effect of the molecular environment: application to a complex
 of p-amino-p&#x2032;-nitrobiphenyl with triphenylphosphine oxide
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2425
_journal_paper_doi               10.1039/a907473b
_journal_year                    1999
_chemical_formula_sum            'C30 H25 N2 O3 P'
_chemical_formula_weight         492.49
_chemical_name_common
;
triphenylphosphine oxide p-amino-p'-nitrobiphenyl
;
_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                106.122(4)
_cell_angle_beta                 107.714(5)
_cell_angle_gamma                94.691(4)
_cell_formula_units_Z            2
_cell_length_a                   9.2719(8)
_cell_length_b                   10.4330(10)
_cell_length_c                   14.4569(11)
_cell_measurement_reflns_used    800
_cell_measurement_temperature    90(1)
_cell_measurement_theta_max      52.27
_cell_measurement_theta_min      2.07
_cell_volume                     1258.5(2)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(1)
_diffrn_measured_fraction_theta_full 0.452
_diffrn_measured_fraction_theta_max 0.452
_diffrn_measurement_device_type  'SMART CCD 1K'
_diffrn_measurement_method       'oscillation around \w axis'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0420
_diffrn_reflns_av_sigmaI/netI    0.0644
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            89125
_diffrn_reflns_theta_full        52.27
_diffrn_reflns_theta_max         52.27
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'orange red'
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             516
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.0239(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     426
_refine_ls_number_reflns         13140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.0497
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0344P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                16028
_reflns_number_total             27997
_reflns_threshold_expression     >4sigma(I)
_cod_data_source_file            907473bsup1.cif
_cod_data_source_block           tppopanb
_cod_original_cell_volume        1258.47(19)
_cod_database_code               7110718