Amidine functionalized phosphines: tuneable ligands for transition metals
Newman, Paul David; Melen, Rebecca; Platts, James A.; Wilkins, Lewis; Dalton Trans.  (2017) –; doi:10.1039/C7DT03343E

data_7044398
_publ_section_title
;
 Amidine functionalized phosphines: tuneable ligands for transition metals
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT03343E
_journal_year                    2017
_chemical_absolute_configuration as
_chemical_formula_moiety         'C20 H34 N2 O3 P, B F4'
_chemical_formula_sum            'C20 H34 B F4 N2 O3 P'
_chemical_formula_weight         468.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-06-20 deposited with the CCDC.
2017-10-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.808(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4905(5)
_cell_length_b                   7.7502(2)
_cell_length_c                   15.2759(4)
_cell_measurement_reflns_used    6096
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5670
_cell_measurement_theta_min      4.5150
_cell_volume                     2291.23(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41g (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41g (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41g (Rigaku OD, 2015)'
_computing_molecular_graphics    'XSHELL and Mercury'
_computing_publication_material  XCIF
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Agilent Supernova Dual Atlas w/ CCD detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0605
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15730
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.500
_diffrn_reflns_theta_min         3.482
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.956
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41g (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model Empirical absorption correction using 
spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       block
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.04(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8248
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0713
_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^)+(0.1298P)^2^+1.1459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1938
_refine_ls_wR_factor_ref         0.2058
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                7202
_reflns_number_total             8248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03343e2.cif
_cod_data_source_block           rm1702d
_cod_original_cell_volume        2291.25(11)
_cod_database_code               7044398
_shelx_estimated_absorpt_t_min   0.704
_shelx_estimated_absorpt_t_max   0.908
_shelxl_version_number           2013-3
_shelx_res_checksum              71374