Platinum(ii) complexes of mixed-valent radicals derived from cyclotricatechylene, a macrocyclic tris-dioxolene
Loughrey, Jonathan J.; Patmore, Nathan J.; Baldansuren, Amgalanbaatar; Fielding, Alistair J.; McInnes, Eric J. L.; Hardie, Michaele J.; Sproules, Stephen; Halcrow, Malcolm A.; Chem. Sci. 6 (2015) 6935–; doi:10.1039/C5SC02776D

data_1529425
_publ_section_title
;
 Platinum(ii) complexes of mixed-valent radicals derived from
 cyclotricatechylene, a macrocyclic tris-dioxolene
;
_journal_issue                   12
_journal_name_full               'Chem. Sci.'
_journal_page_first              6935
_journal_paper_doi               10.1039/C5SC02776D
_journal_volume                  6
_journal_year                    2015
_chemical_formula_moiety         'C99 H84 O6 P6 Pt3, H2 O, 8[C4 H9 N O]'
_chemical_formula_sum            'C131 H158 N8 O15 P6 Pt3'
_chemical_formula_weight         2855.74
_chemical_name_systematic
; 
Tris[(1,2-bis{diphenylphosphinoethane}platinum(II)]cyclotricatechylene
hydrate octakis-dimethylacetamide solvate
;
_space_group_IT_number           176
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   23.8013(6)
_cell_length_b                   23.8013(6)
_cell_length_c                   13.6022(5)
_cell_measurement_reflns_used    66070
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.98
_cell_volume                     6673.3(3)
_computing_cell_refinement
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_collection
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_data_reduction
'CrystalClear-SM Expert 2.0 rc13 (Rigaku, 2009)'
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku Saturn CCD'
_diffrn_measurement_method       'profile data from \w scans'
_diffrn_radiation_monochromator  silicon
_diffrn_radiation_source         'Diamond Light Source station I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.69980
_diffrn_reflns_av_R_equivalents  0.0827
_diffrn_reflns_av_sigmaI/netI    0.0345
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            66070
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.270
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS (Sheldrick, 2002).  University of Gottingen, Germany.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.444
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.203
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         5308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.203
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0803
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+151.4837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1886
_refine_ls_wR_factor_ref         0.1897
_reflns_number_gt                5132
_reflns_number_total             5308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc02776d2.cif
_cod_data_source_block           jjl95b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Hexagonal' changed to 'hexagonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1529425--1529426.cif.
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_cod_database_code               1529425