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_7122433
_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         'C29 H36 B Mo N6 O2 P Si'
_chemical_formula_sum            'C29 H36 B Mo N6 O2 P Si'
_chemical_formula_weight         666.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0572(4)
_cell_length_b                   10.5503(2)
_cell_length_c                   17.9411(4)
_cell_measurement_reflns_used    14075
_cell_measurement_temperature    150.01(1)
_cell_measurement_theta_max      28.0630
_cell_measurement_theta_min      3.7910
_cell_volume                     3228.65(12)
_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)'
_diffrn_ambient_temperature      150.01(1)
_diffrn_detector_area_resol_mean 10.3744
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.883
_diffrn_measurement_device_type  'New Xcalibur, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0323
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.883
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            28899
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.816
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.892
_diffrn_reflns_theta_min         3.275
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.528
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98803
_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            yellow
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.414
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.129
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Flack x determined using 2648 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(12)
_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     383
_refine_ls_number_reflns         6939
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0312P)^2^+1.4771P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0696
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    0.949
_reflns_Friedel_fraction_max     0.745
_reflns_number_gt                6359
_reflns_number_total             6939
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc07166g2.cif
_cod_data_source_block           Compound_2a
_cod_depositor_comments
'Adding full bibliography for 7122430--7122440.cif.'
_cod_database_code               7122433
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              3775
_shelx_hkl_checksum              62694