Sterically-constrained tripodal phosphorus-bridged tris-pyridyl ligands.
Hanf, Schirin; García-Rodríguez, Raúl; Bond, Andrew D.; Hey-Hawkins, Evamarie; Wright, Dominic S.; Dalton transactions (Cambridge, England : 2003) 45 (2015) 276–283; doi:10.1039/c5dt04155d

data_7037283
_publ_section_title
;
 Sterically-constrained tripodal phosphorus-bridged tris-pyridyl ligands.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              276
_journal_page_last               283
_journal_paper_doi               10.1039/c5dt04155d
_journal_volume                  45
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C15 H9 Br3 N3 P'
_chemical_formula_sum            'C15 H9 Br3 N3 P'
_chemical_formula_weight         501.95
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-10-16 deposited with the CCDC.
2015-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   15.7876(6)
_cell_length_b                   15.7876(6)
_cell_length_c                   11.1637(5)
_cell_measurement_reflns_used    4282
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.62
_cell_measurement_theta_min      5.60
_cell_volume                     2409.74(17)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0622
_diffrn_reflns_av_unetI/netI     0.0368
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7384
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        66.738
_diffrn_reflns_theta_max         66.738
_diffrn_reflns_theta_min         5.604
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    10.247
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.075
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details
;
Flack x determined using 393 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         941
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0142P)^2^+16.7202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0609
_refine_ls_wR_factor_ref         0.0624
_reflns_Friedel_coverage         0.965
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                873
_reflns_number_total             941
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt04155d2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7037282--7037287.cif.'
_cod_original_cell_volume        2409.7(2)
_cod_database_code               7037283
_shelx_estimated_absorpt_t_min   0.211
_shelx_estimated_absorpt_t_max   0.628
_shelx_res_checksum              70390