Zirconium-catalyzed intermolecular hydrophosphination using a chiral, air-stable primary phosphine.
Bange, Christine A.; Ghebreab, Michael B.; Ficks, Arne; Mucha, Neil T.; Higham, Lee; Waterman, Rory; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1863–1867; doi:10.1039/c5dt03544a

data_7038142
_publ_section_title
;
 Zirconium-catalyzed intermolecular hydrophosphination using a chiral,
 air-stable primary phosphine.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1863
_journal_page_last               1867
_journal_paper_doi               10.1039/c5dt03544a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_sum            'C36 H55 N4 O P Si3 Zr'
_chemical_formula_weight         766.29
_chemical_name_common            Binolphosphine
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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   mixed
_audit_update_record
;
2015-10-13 deposited with the CCDC.
2015-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                77.714(2)
_cell_angle_beta                 81.478(2)
_cell_angle_gamma                71.588(2)
_cell_formula_units_Z            2
_cell_length_a                   10.843(2)
_cell_length_b                   12.324(2)
_cell_length_c                   18.699(3)
_cell_measurement_reflns_used    8388
_cell_measurement_temperature    128.(2)
_cell_measurement_theta_max      26.3039
_cell_measurement_theta_min      2.1943
_cell_volume                     2307.7(7)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      128.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0679
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16718
_diffrn_reflns_theta_full        21.89
_diffrn_reflns_theta_max         21.89
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.400
_refine_ls_abs_structure_details
;
Flack x determined using 3984 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.11(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     837
_refine_ls_number_reflns         10948
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1327
_reflns_number_gt                9213
_reflns_number_total             10948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt03544a2.cif
_cod_data_source_block           I
_cod_database_code               7038142
_shelx_res_checksum              91907