Increasing steric demand through flexible bulk - primary phosphanes with 2,6-bis(benzhydryl)phenyl backbones.
Bresien, Jonas; Goicoechea, Jose M.; Hinz, Alexander; Scharnhölz, Moritz T; Schulz, Axel; Suhrbier, Tim; Villinger, Alexander; Dalton transactions (Cambridge, England : 2003) 48 (2019) 3786–3794; doi:10.1039/c9dt00399a

data_7049101
_publ_section_title
;
 Increasing steric demand through flexible bulk - primary phosphanes with
 2,6-bis(benzhydryl)phenyl backbones.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3786
_journal_page_last               3794
_journal_paper_doi               10.1039/c9dt00399a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '0.885(C33 H27 Cl2 Sb), 0.115(C33 H27 I2 Sb)'
_chemical_formula_sum            'C33 H27 Cl1.77 I0.23 Sb'
_chemical_formula_weight         636.85
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-01-28 deposited with the CCDC.    2019-02-20 downloaded from the CCDC.
;
_cell_angle_alpha                104.561(4)
_cell_angle_beta                 106.008(4)
_cell_angle_gamma                109.385(4)
_cell_formula_units_Z            2
_cell_length_a                   9.5535(9)
_cell_length_b                   12.4822(12)
_cell_length_c                   13.5312(13)
_cell_measurement_reflns_used    9982
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      26.10
_cell_measurement_theta_min      2.36
_cell_volume                     1354.4(2)
_computing_cell_refinement       'Bruker Apex3 2017.3'
_computing_data_collection       'Bruker Apex3 2017.3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker Kappa Apex-II CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_unetI/netI     0.0472
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_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            82814
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.500
_diffrn_reflns_theta_min         2.361
_exptl_absorpt_coefficient_mu    1.471
_exptl_absorpt_correction_T_max  0.7472
_exptl_absorpt_correction_T_min  0.6893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.537
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         9811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0363
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0192P)^2^+1.5263P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0765
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8009
_reflns_number_total             9811
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00399a2.cif
_cod_data_source_block           is_ms432
_cod_depositor_comments
'Adding full bibliography for 7049097--7049105.cif.'
_cod_database_code               7049101
_shelx_estimated_absorpt_t_min   0.820
_shelx_estimated_absorpt_t_max   0.917
_shelxl_version_number           2013-4
_shelx_res_checksum              34426