Convenient Synthesis of a Highly Soluble and Stable Phosphorescent Platinum Porphyrin Dye
Zems, Yaroslav; Moiseev, Andrey G.; Perepichka, Dmitrii F.; Organic Letters 15 (2013) 5330–; doi:10.1021/ol402590c

data_1512583
_publ_section_title
;
 Convenient Synthesis of a Highly Soluble and Stable Phosphorescent
 Platinum Porphyrin Dye
;
_journal_issue                   20
_journal_name_full               'Organic Letters'
_journal_page_first              5330
_journal_paper_doi               10.1021/ol402590c
_journal_volume                  15
_journal_year                    2013
_chemical_absolute_configuration rmad
_chemical_compound_source        'Synthesized by the authors. See text'
_chemical_formula_moiety         'C100 H96 N8 O8 Pt'
_chemical_formula_sum            'C100 H96 N8 O8 Pt'
_chemical_formula_weight         1732.93
_space_group_crystal_system      tetragonal
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.2352(8)
_cell_length_b                   21.2352(8)
_cell_length_c                   23.791(1)
_cell_measurement_reflns_used    9670
_cell_measurement_temperature    150
_cell_measurement_theta_max      70.07
_cell_measurement_theta_min      4.17
_cell_volume                     10728.2(7)
_computing_cell_refinement       'SAINT V8.30C(Bruker AXS, 2013)'
_computing_data_collection       'APEX2  (Bruker AXS, 2013)'
_computing_data_reduction        'SAINT V8.30C(Bruker AXS, 2013)'
_computing_molecular_graphics    'XP  (Bruker AXS, 1998)'
_computing_publication_material  'UdMX (Maris, 2004)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Microstar'
_diffrn_measurement_method       \w
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_av_unetI/netI     0.0202
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            124268
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.398
_diffrn_reflns_theta_min         4.164
_diffrn_source                   'Rotating Anode'
_exptl_absorpt_coefficient_mu    2.844
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.6090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2012)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_description       block
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
Attempts to  model disordered solvent molecules
were unsuccessful. PLATON/SQUEEZE  was used to correct
the data for the presence of the disordered solvent.
A potential solvent volume of 2817.9 \%A^3^, 
26.3 % of the total unit-cell volume, was found.
 electrons per unit cell worth of scattering were located
in the void. The reported structure is based on the 
PLATON/SQUEEZE corrected data. The actual solvent content is
unknown, so several quantities calculated like empirical formula, density, 
absorption coefficient, F(000) etc. may be incorrect.

Ref:  Sluis, P. van der & Spek, A.L. (1990). Acta Cryst. A46, 194-201.
;
_refine_diff_density_max         1.023
_refine_diff_density_min         -2.468
_refine_diff_density_rms         0.117
_refine_ls_abs_structure_details
;
 Flack x determined using 2274 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.065(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.196
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5088
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.183
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+7.1072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1151
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                5025
_reflns_number_total             5088
_cod_data_source_file            ol402590c_si_002.cif
_cod_data_source_block           PERE41
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_absolute_configuration' value 'RMAD' changed to 'rmad'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        10728.2(9)
_cod_original_sg_symbol_H-M      I-42d
_cod_database_code               1512583
_shelx_estimated_absorpt_t_min   0.483
_shelx_estimated_absorpt_t_max   0.675