Photocrystallisation of the 2C–2′C dimer of a triphenylimidazolyl radical
Edkins, Robert M.; Probert, Michael R.; Robertson, Craig M.; Howard, Judith A. K.; Beeby, Andrew; RSC Adv. 4 (2014) 5351–; doi:10.1039/C3RA43892A

data_7239241
_publ_section_title
;
 Photocrystallisation of the 2C--2&#x2032;C dimer of a triphenylimidazolyl
 radical
;
_journal_issue                   11
_journal_name_full               'RSC Adv.'
_journal_page_first              5351
_journal_paper_doi               10.1039/C3RA43892A
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C33 H28 N2, 2(C2 H6 O)'
_chemical_formula_sum            'C37 H40 N2 O2'
_chemical_formula_weight         544.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2013-11-27
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2013.11.15 svn.r2839 for OlexSys, GUI svn.r4715)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.424(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0885(12)
_cell_length_b                   29.010(3)
_cell_length_c                   9.9651(10)
_cell_measurement_reflns_used    914
_cell_measurement_temperature    120.0
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      2.52
_cell_volume                     3130.5(6)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20707
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.407
_diffrn_reflns_theta_min         1.404
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.894290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0307 before and 0.0237 after correction.
The Ratio of minimum to maximum transmission is 0.8943.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.298
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     381
_refine_ls_number_reflns         6420
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0783
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0571P)^2^+1.5441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1226
_refine_ls_wR_factor_ref         0.1339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4754
_reflns_number_total             6420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c3ra43892a.txt
_cod_data_source_block           final
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_source_target' value 'MO' was changed to 'Mo' in
accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3130.4(6)
_cod_database_code               7239241
_shelxl_version_number           2013-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C5S(H5SA,H5SB)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C10(H10), C11(H11), C15(H15), C16(H16), C18(H18), C19(H19),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35)
2.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C1S(H1SA,H1SB,
 H1SC), C4S(H4SA,H4SB,H4SC)
2.d Idealised tetrahedral OH refined as rotating group:
 O3S(H3S), O6S(H6S)
;
_shelx_res_checksum              50767
_shelx_hkl_checksum              66344