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_7043364
_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         'C33 H56 B I N6 O P2 W'
_chemical_formula_sum            'C33 H56 B I N6 O P2 W'
_chemical_formula_weight         936.33
_chemical_name_systematic
'[\h2-C,C?-{bis(diisopropylphosphanyl)acetylene}(carbonyl){hydridotris(3,4,5-trimethylpyrazolyl)borate}(iodido)-tungsten(II)]'
_chemical_properties_physical    ', Air-sensitive,Oxygen-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2017-03-30 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                100.6510(10)
_cell_angle_beta                 102.567(2)
_cell_angle_gamma                104.2780(10)
_cell_formula_units_Z            2
_cell_length_a                   10.7720(3)
_cell_length_b                   10.9323(3)
_cell_length_c                   18.1301(6)
_cell_measurement_reflns_used    9891
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.61
_cell_measurement_theta_min      2.38
_cell_volume                     1954.28(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    Mercury
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            64275
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.499
_diffrn_reflns_theta_min         1.986
_exptl_absorpt_coefficient_mu    3.860
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.5757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       block
_exptl_crystal_F_000             932
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, n-pentane'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.110
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         14059
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0252
_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^)+(0.0255P)^2^+1.7392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12419
_reflns_number_total             14059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01803g2.cif
_cod_data_source_block           kh307
_cod_database_code               7043364
_shelx_estimated_absorpt_t_min   0.458
_shelx_estimated_absorpt_t_max   0.711
_shelxl_version_number           2014-3
_shelx_res_checksum              4738