Alkynylbis(alkylidynyl)phosphines: {L<sub>n</sub>M[triple bond, length as m-dash]C}<sub>2</sub>PC[triple bond, length as m-dash]CR.
Frogley, Benjamin J.; Hill, Anthony F.; Chemical communications (Cambridge, England) 54 (2018) 12373–12376; doi:10.1039/c8cc07166g

data_7122431
_publ_section_title
;
 Alkynylbis(alkylidynyl)phosphines: {L<sub>n</sub>M[triple bond, length as
 m-dash]C}<sub>2</sub>PC[triple bond, length as m-dash]CR.
;
_journal_issue                   87
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              12373
_journal_page_last               12376
_journal_paper_doi               10.1039/c8cc07166g
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C38 H45 B2 N12 O4 P W2'
_chemical_formula_sum            'C38 H45 B2 N12 O4 P W2'
_chemical_formula_weight         1154.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-06-27 deposited with the CCDC.
2018-10-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.766(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.2850(6)
_cell_length_b                   10.7644(5)
_cell_length_c                   27.3927(10)
_cell_measurement_reflns_used    6452
_cell_measurement_temperature    150.0(1)
_cell_measurement_theta_max      28.2530
_cell_measurement_theta_min      3.8390
_cell_volume                     4497.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      150.0(1)
_diffrn_detector_area_resol_mean 8.1297
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0406
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            14491
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.318
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.199
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       plate
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.126
_exptl_crystal_size_mid          0.115
_exptl_crystal_size_min          0.021
_refine_diff_density_max         1.899
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         4587
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0430
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0370P)^2^+5.8432P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0753
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3737
_reflns_number_total             4587
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07166g2.cif
_cod_data_source_block           Compound_10
_cod_depositor_comments
'Adding full bibliography for 7122430--7122440.cif.'
_cod_database_code               7122431
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              56666
_shelx_hkl_checksum              31376