Synthesis, crystallization, electrochemistry and single crystal X-ray analysis of a methoxy-substituted-tris-phenalenyl based neutral radical
Sarkar, Arindam; Tham, Fook S.; Haddon, Robert C.; Journal of Materials Chemistry 21 (2011) 1574–; doi:10.1039/c0jm02397c

data_7205547
_publ_section_title
;
 Synthesis, crystallization, electrochemistry and single crystal X-ray
 analysis of a methoxy-substituted-tris-phenalenyl based neutral
 radical
;
_journal_issue                   5
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1574
_journal_paper_doi               10.1039/c0jm02397c
_journal_volume                  21
_journal_year                    2011
_chemical_formula_sum            'C50.83 H41.74 N2.91 O12 Si'
_chemical_formula_weight         913.48
_chemical_name_systematic
;

?

;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.192(3)
_cell_angle_beta                 104.382(3)
_cell_angle_gamma                101.723(3)
_cell_formula_units_Z            2
_cell_length_a                   12.357(2)
_cell_length_b                   12.711(2)
_cell_length_c                   14.644(3)
_cell_measurement_reflns_used    2232
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.79
_cell_measurement_theta_min      2.26
_cell_volume                     2175.4(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0970
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20412
_diffrn_reflns_theta_full        20.39
_diffrn_reflns_theta_max         20.39
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.126
_exptl_absorpt_correction_T_max  0.9987
_exptl_absorpt_correction_T_min  0.9741
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin plate frag'
_exptl_crystal_F_000             954
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.339
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     613
_refine_ls_number_reflns         4292
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0641P)^2^+2.9307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1563
_reflns_number_gt                2587
_reflns_number_total             4292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0JM02397C.TXT
_cod_data_source_block           rh141_0m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 1555 2011-01-17 13:19:09Z saulius 

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-1
_cod_database_code               7205547