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_7043367
_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         'C39 H52 B Cl2 I N6 O P2 Pt W, 2(C H2 Cl2)'
_chemical_formula_sum            'C40.92 H55.88 B Cl5.89 I N6 O P2 Pt W'
_chemical_formula_weight         1435.10
_chemical_name_systematic
syn-{\m-(diisopropylphosphanyl)(diphenylphosphanyl)acetylene}-[(carbonyl){hydridotris(3,4,5-trimethylpyrazolyl)borate}(iodido)-\h2-C,C?-tungsten(II)]-[dichlorido-\k2-P,P?-platinum(II)]
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                90
_cell_angle_beta                 115.980(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5361(6)
_cell_length_b                   25.7551(10)
_cell_length_c                   15.0081(6)
_cell_measurement_reflns_used    9775
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      32.63
_cell_measurement_theta_min      2.27
_cell_volume                     5050.9(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0567
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            90447
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.500
_diffrn_reflns_theta_min         2.269
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    6.074
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.5446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.910
_exptl_crystal_description       block
_exptl_crystal_F_000             2800
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, diethylether'
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.121
_refine_diff_density_min         -1.428
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     583
_refine_ls_number_reflns         18268
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0260
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0167P)^2^+4.6052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15563
_reflns_number_total             18268
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01803g2.cif
_cod_data_source_block           kh_sd23
_cod_database_code               7043367
_shelx_estimated_absorpt_t_min   0.281
_shelx_estimated_absorpt_t_max   0.676
_shelxl_version_number           2014-3
_shelx_res_checksum              72844