The Synthesis of New 60° Organometallic Subunits and Self-Assembly of Three-Dimensional M~3~L~2~ Trigonal-Bipyramidal Cages
Hai-Bo Yang; Koushik Ghosh; Atta M. Arif; Peter J. Stang; Journal of Organic Chemistry 71 (2006) 9464–9469; doi:10.1021/jo061779j

data_4022158
_publ_section_title
;
 The Synthesis of New 60\% Organometallic Subunits and
 Self-Assembly of Three-Dimensional M~3~L~2~
 Trigonal-Bipyramidal Cages
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9464
_journal_page_last               9469
_journal_paper_doi               10.1021/jo061779j
_journal_volume                  71
_journal_year                    2006
_chemical_formula_moiety         'C58 H76 I2 P4 Pt2,1.5(C1 H2 Cl2)'
_chemical_formula_sum            'C59.5 H79 Cl3 I2 P4 Pt2'
_chemical_formula_weight         1668.44
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.3871(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   42.0070(6)
_cell_length_b                   9.3291(2)
_cell_length_c                   34.7621(6)
_cell_measurement_reflns_used    8938
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      1.018
_cell_volume                     12850.4(4)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'WinGX, Ortep3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Nonius KappaCCD Diffractometer'
_diffrn_measurement_method       'Phi and Omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -51
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            20462
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.03
_exptl_absorpt_coefficient_mu    5.570
_exptl_absorpt_correction_T_max  0.6642
_exptl_absorpt_correction_T_min  0.3365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO-SMN (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.725
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6472
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.395
_refine_diff_density_min         -1.873
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         12134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0653P)^2^+185.2146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1454
_reflns_number_gt                8609
_reflns_number_total             12134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo061779jsi20060829_115018.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C59.50 H79 Cl3 I2 P4 Pt2'
_cod_database_code               4022158