Self-assembly of 2∶2 and 3∶3 metallamacrocyclic complexes of platinum(II) with symmetrical, bipodal N′,N′,N ‴N ‴-tetraalkyl-N,N ″-phenylenedicarbonylbis(thiourea)
Koch, Klaus R.; Bourne, Susan A.; Coetzee, Anita; Miller, Jörn; Journal of the Chemical Society, Dalton Transactions  (1999) 3157–; doi:10.1039/a904181h

data_7027571
_publ_section_title
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 Self-assembly of 2&#x2236;2 and 3&#x2236;3 metallamacrocyclic complexes
 of platinum(II) with symmetrical, bipodal
 N&#x2032;,N&#x2032;,N&#x200A;&#x2034;N&#x200A;&#x2034;-tetraalkyl-N,N&#x200A;&#x2033;-phenylenedicarbonylbis(thiourea)
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_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3157
_journal_paper_doi               10.1039/a904181h
_journal_year                    1999
_chemical_formula_moiety         'C78 H120 N12 O6 Pt3 S6,2(CHCl3),C2H6O,2H2O'
_chemical_formula_sum            'C82 H132 Cl6 N12 O9 Pt3 S6'
_chemical_formula_weight         2420.41
_chemical_melting_point_gt       593.15
_chemical_name_systematic
; 
cis-tris-(3,3,3',3'-tetrabutyl-1,1'-terephthaloyl-bis(thiourea))platinum(II)' 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.261(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.611(1)
_cell_length_b                   23.293(2)
_cell_length_c                   26.033(1)
_cell_measurement_reflns_used    25108
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.96
_cell_volume                     10649.6(12)
_computing_cell_refinement       DENZO
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        SCALEPACK
_computing_molecular_graphics    PLUTO
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            25105
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    4.253
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.690
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   Scalepack
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4944
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.406
_refine_diff_density_min         -1.551
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     758
_refine_ls_number_reflns         25105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0617
_refine_ls_shift/su_max          1.209
_refine_ls_shift/su_mean         0.235
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0992P)^2^+42.0709P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1713
_refine_ls_wR_factor_ref         0.1972
_reflns_number_gt                17609
_reflns_number_total             25105
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904181Hsup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>320\%C' was changed to
'593.15' - it was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7027571