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_7118959
_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
'C216 H180 Br4 Fe6 N12 O12 P12 Pt4, 4(Br), 21(C H Cl3)'
_chemical_formula_sum            'C237 H201 Br8 Cl63 Fe6 N12 O12 P12 Pt4'
_chemical_formula_weight         7768.82
_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_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2016-04-18 deposited with the CCDC.
2016-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                88.034(3)
_cell_angle_beta                 89.129(3)
_cell_angle_gamma                65.458(2)
_cell_formula_units_Z            2
_cell_length_a                   21.46830(10)
_cell_length_b                   23.59400(10)
_cell_length_c                   32.9537(8)
_cell_measurement_reflns_used    27167
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      2.9794
_cell_measurement_wavelength     0.71075
_cell_volume                     15174.9(5)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 7.32
_diffrn_measured_fraction_theta_full 0.859
_diffrn_measured_fraction_theta_max 0.859
_diffrn_measurement_details
;
scan:
    Number of images: 1800
               Slice: -80.0000 - 100.0000
         Image width: 0.1000
            Exp time: 24.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 75.1584
              2theta: 30.1144
scan:
    Number of images: 540
               Slice: -10.0000 - 44.0000
         Image width: 0.1000
            Exp time: 24.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 75.1584
              2theta: 30.1144
scan:
    Number of images: 540
               Slice: -10.0000 - 44.0000
         Image width: 0.1000
            Exp time: 24.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 75.1584
              2theta: 30.1144
scan:
    Number of images: 540
               Slice: -10.0000 - 44.0000
         Image width: 0.1000
            Exp time: 24.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 75.1584
              2theta: 30.1144
scan:
    Number of images: 540
               Slice: -10.0000 - 44.0000
         Image width: 0.1000
            Exp time: 24.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 270.0000
                 XTD: 75.1584
              2theta: 30.1144

;
_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     0.71075
_diffrn_reflns_av_R_equivalents  0.0327
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 0.859
_diffrn_reflns_Laue_measured_fraction_max 0.859
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            75372
_diffrn_reflns_point_group_measured_fraction_full 0.859
_diffrn_reflns_point_group_measured_fraction_max 0.859
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.887
_diffrn_source_current           250.0000
_diffrn_source_power             13.7500
_diffrn_source_voltage           55.0000
_exptl_absorpt_coefficient_mu    3.839
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8177
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             7604
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         3.206
_refine_diff_density_min         -2.338
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2719
_refine_ls_number_reflns         45899
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0700
_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^)+(0.1119P)^2^+74.3789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1895
_refine_ls_wR_factor_ref         0.2063
_reflns_number_gt                36867
_reflns_number_total             45899
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc01448h2.cif
_cod_data_source_block           ISEKI-PtBr4-New4
_cod_original_cell_volume        15174.8(5)
_cod_database_code               7118959
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.392
_shelx_estimated_absorpt_t_max   0.447
_shelx_res_checksum              28206
_shelx_fab_checksum              45283