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_7118957
_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         'C72 H60 Fe2 N4 O4 P4 Pt, 4(C H2 Cl2)'
_chemical_formula_sum            'C76 H68 Cl8 Fe2 N4 O4 P4 Pt'
_chemical_formula_weight         1815.61
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_audit_update_record
;
2016-03-29 deposited with the CCDC.
2016-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.950(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.1376(18)
_cell_length_b                   15.0037(8)
_cell_length_c                   18.0317(12)
_cell_measurement_reflns_used    7954
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.4758
_cell_measurement_theta_min      2.1091
_cell_volume                     7409.9(8)
_computing_cell_refinement       'CrystalClear (Rigaku, 2001)'
_computing_data_collection       'CrystalClear (Rigaku, 2001)'
_computing_data_reduction        'CrystalClear (Rigaku, 2001)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  SHELXL97
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
scan:
    Number of images: 1200
               Slice: -80.0000 - 100.0000
         Image width: 0.1500
            Exp time: 8.0000
       Rotation axis: Phi
               Omega: 0.0000
                 Chi: 0.0000
                 Phi: 0.0000
                 XTD: 55.2375
              2theta: 25.1388
scan:
    Number of images: 400
               Slice: -15.0000 - 45.0000
         Image width: 0.1500
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 0.0000
                 XTD: 55.2375
              2theta: 25.1388
scan:
    Number of images: 400
               Slice: -15.0000 - 45.0000
         Image width: 0.1500
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 90.0000
                 XTD: 55.2375
              2theta: 25.1388
scan:
    Number of images: 400
               Slice: -15.0000 - 45.0000
         Image width: 0.1500
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 180.0000
                 XTD: 55.2375
              2theta: 25.1388
scan:
    Number of images: 400
               Slice: -15.0000 - 45.0000
         Image width: 0.1500
            Exp time: 8.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 90.0000
                 Phi: 270.0000
                 XTD: 55.2375
              2theta: 25.1388

;
_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  0.0437
_diffrn_reflns_av_unetI/netI     0.0428
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28446
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.36
_diffrn_source_current           250.0000
_diffrn_source_power             12.5000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    2.697
_exptl_absorpt_correction_T_max  0.7742
_exptl_absorpt_correction_T_min  0.7206
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Platelet
_exptl_crystal_F_000             3640
_exptl_crystal_preparation
'mounted on the CryoLoop with Palaton oil and placed in N2 stream at 200(2) K'
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.868
_refine_diff_density_min         -1.151
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         8452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0345P)^2^+31.3545P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                7530
_reflns_number_total             8452
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc01448h2.cif
_cod_data_source_block           ISK-372-New
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7118957