Tetrahedral cage complex with planar vertices: selective synthesis of Pt4L6 cage complexes involving hydrogen bonds driven by halide binding
Masaki Ito; Masato Iseki; Masumi Itazaki; Hiroshi Nakazawa; Chem.Commun. 52 (2016) 7205–; doi:

data_7118960
_publ_section_title
;
 Tetrahedral cage complex with planar vertices: selective synthesis of
 Pt4L6 cage complexes involving hydrogen bonds driven by halide binding
;
_journal_name_full               Chem.Commun.
_journal_page_first              7205
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C57 H48 Cl N3 O3 P3 Pt, Cl, C4 H10 O'
_chemical_formula_sum            'C61 H58 Cl2 N3 O4 P3 Pt'
_chemical_formula_weight         1256.00
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_update_record
;
2016-03-29 deposited with the CCDC.
2016-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                83.953(3)
_cell_angle_beta                 73.888(3)
_cell_angle_gamma                87.375(2)
_cell_formula_units_Z            2
_cell_length_a                   11.79990(10)
_cell_length_b                   12.6886(2)
_cell_length_c                   19.4168(2)
_cell_measurement_reflns_used    7234
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.0373
_cell_volume                     2777.02(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_publication_material  'Yadokari-XG (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>,  1999)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
scan:
    Number of images: 600
               Slice: -80.0000 - 100.0000
         Image width: 0.3000
            Exp time: 4.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 55.0398
              2theta: 24.9543
scan:
    Number of images: 200
               Slice: -15.0000 - 45.0000
         Image width: 0.3000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 55.0398
              2theta: 24.9543
scan:
    Number of images: 200
               Slice: -15.0000 - 45.0000
         Image width: 0.3000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 55.0398
              2theta: 24.9543
scan:
    Number of images: 200
               Slice: -15.0000 - 45.0000
         Image width: 0.3000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 55.0398
              2theta: 24.9543
scan:
    Number of images: 200
               Slice: -15.0000 - 45.0000
         Image width: 0.3000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 270.0000
                 XTD: 55.0398
              2theta: 24.9543
scan:
    Number of images: 195
               Slice: -15.0000 - 43.5000
         Image width: 0.3000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 55.0398
              2theta: 24.9543
scan:
    Number of images: 195
               Slice: -15.0000 - 43.5000
         Image width: 0.3000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 55.0398
              2theta: 24.9543
scan:
    Number of images: 195
               Slice: -15.0000 - 43.5000
         Image width: 0.3000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 55.0398
              2theta: 24.9543
scan:
    Number of images: 195
               Slice: -15.0000 - 43.5000
         Image width: 0.3000
            Exp time: 4.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 55.0398
              2theta: 24.9543

;
_diffrn_measurement_device       'Mercury CCD (2x2 bin mode)'
_diffrn_measurement_device_details 'AFC7: Eulerian 3-circle'
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Graphite Monochromator'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            31987
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.35
_diffrn_source_current           200.0000
_diffrn_source_power             10.0000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.759
_exptl_absorpt_correction_T_max  0.6823
_exptl_absorpt_correction_T_min  0.4915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            'Pale Yellow'
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1268
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.575
_refine_diff_density_min         -0.814
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         12208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_gt           0.0301
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0274P)^2^+2.5318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                11353
_reflns_number_total             12208
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc01448h2.cif
_cod_data_source_block           ITM-1017-New
_cod_original_cell_volume        2777.02(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7118960