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_1529426
_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, 2.04[H2 O], 0.5 [C H4 O], 1.3[C4 H9 N O]'
_chemical_formula_sum            'C104.7 H101.78 N1.3 O9.84 P6 Pt3'
_chemical_formula_weight         2306.78
_chemical_name_systematic
; 
Tris[(1,2-bis{diphenylphosphinoethane}platinum(II)]cyclotricatechylene
dihydrate dimethylacetamide (2/1.3) methanol (1/0.5) solvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 98.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   14.860(3)
_cell_length_b                   23.898(5)
_cell_length_c                   15.103(3)
_cell_measurement_reflns_used    51623
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.70
_cell_measurement_theta_min      1.61
_cell_volume                     5299.3(19)
_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 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0389
_diffrn_reflns_av_sigmaI/netI    0.0619
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            51623
_diffrn_reflns_theta_full        27.70
_diffrn_reflns_theta_max         27.70
_diffrn_reflns_theta_min         1.61
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.094
_exptl_absorpt_correction_T_max  0.889
_exptl_absorpt_correction_T_min  0.803
_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    1.446
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular prism'
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.735
_refine_diff_density_min         -1.561
_refine_diff_density_rms         0.166
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.009(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     896
_refine_ls_number_reflns         20525
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0828P)^2^+3.5816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                17240
_reflns_number_total             20525
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5sc02776d2.cif
_cod_data_source_block           jjl95b1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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.
;
_cod_original_cell_volume        5299.1(18)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C104.70 H101.78 N1.30 O9.84 P6 Pt3'
_cod_database_code               1529426