P, P-Dimethylformylphosphine: The Phosphorus Analogue of N, N-Dimethylformamide.
Szkop, Kevin M.; Jupp, Andrew R.; Stephan, Douglas W.; Journal of the American Chemical Society 140 (2018) 12751–12755; doi:10.1021/jacs.8b09266

data_4133284
_publ_section_title
;
 P, P-Dimethylformylphosphine: The Phosphorus Analogue of N,
 N-Dimethylformamide.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12751
_journal_page_last               12755
_journal_paper_doi               10.1021/jacs.8b09266
_journal_volume                  140
_journal_year                    2018
_chemical_formula_sum            'C49 H55 B Ge K O7 P'
_chemical_formula_weight         909.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.553(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.154(2)
_cell_length_b                   11.9170(9)
_cell_length_c                   15.3471(11)
_cell_measurement_reflns_used    5710
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.36
_cell_measurement_theta_min      2.93
_cell_volume                     4549.3(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0962
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            37680
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.520
_diffrn_reflns_theta_min         2.684
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       shard
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         5215
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.165
_refine_ls_R_factor_all          0.1347
_refine_ls_R_factor_gt           0.0767
_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^)+(0.0654P)^2^+20.5437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1954
_refine_ls_wR_factor_ref         0.2087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2923
_reflns_number_total             5215
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b09266_si_001.cif
_cod_data_source_block           aj1
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4133284
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.920
_shelx_estimated_absorpt_t_max   0.959
_shelx_res_checksum              24281
_shelx_hkl_checksum              29604