Sterically Encumbered Metalla-diphosphines: Unlocking Alkyne Rotation by PtII Coordination
Helmdach, Kai; Dörk, Stephan; Villinger, Alexander; Seidel, Wolfram Willy; Dalton Trans.  (2017) –; doi:10.1039/C7DT01803G

data_7043365
_publ_section_title
;
 Sterically Encumbered Metalla-diphosphines: Unlocking Alkyne Rotation by
 PtII Coordination
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01803G
_journal_year                    2017
_chemical_formula_moiety         'C49 H48 B I Mo N6 O5 P2 W'
_chemical_formula_sum            'C49 H48 B I Mo N6 O5 P2 W'
_chemical_formula_weight         1280.37
_chemical_name_systematic
{\m-Bis(diphenylphosphanyl)acetylene}-[(carbonyl){hydridotris(3,4,5-trimethylpyrazolyl)borate}(iodido)-\h2-C,C?-tungsten(II)]-[tetracarbonyl-\k2-P,P?-molybdenum(0)]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-03-30 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.388(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0382(4)
_cell_length_b                   22.1495(6)
_cell_length_c                   16.9858(5)
_cell_measurement_reflns_used    9919
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      32.37
_cell_measurement_theta_min      2.20
_cell_volume                     4890.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury 2016 '
_computing_publication_material  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex Kappa II-CCD-diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            85411
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.500
_diffrn_reflns_theta_min         1.514
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    3.356
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_description       block
_exptl_crystal_F_000             2512
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, n-pentane'
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.923
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         17625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+4.0596P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14426
_reflns_number_total             17625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01803g2.cif
_cod_data_source_block           kh223
_cod_database_code               7043365
_shelx_estimated_absorpt_t_min   0.539
_shelx_estimated_absorpt_t_max   0.850
_shelxl_version_number           2014-3
_shelx_res_checksum              31671