Multivalent dithiafulvenyl functionalization of dendritic oligo(phenylene vinylene)s with an anthraquinodimethane core.
Khadem, Mohammadreza; Zhao, Yuming; Chemical communications (Cambridge, England) 53 (2017) 1821–1824; doi:10.1039/c6cc10085f

data_7119438
_publ_section_title
;
 Multivalent dithiafulvenyl functionalization of dendritic oligo(phenylene
 vinylene)s with an anthraquinodimethane core.
;
_journal_issue                   11
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              1821
_journal_page_last               1824
_journal_paper_doi               10.1039/c6cc10085f
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C44 H28 O4, C4 H8 O2'
_chemical_formula_sum            'C48 H36 O6'
_chemical_formula_weight         708.77
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_creation_date             2016-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-11-21 deposited with the CCDC.
2017-01-13 downloaded from the CCDC.
;
_cell_angle_alpha                95.181(5)
_cell_angle_beta                 103.451(4)
_cell_angle_gamma                101.178(5)
_cell_formula_units_Z            2
_cell_length_a                   10.9553(5)
_cell_length_b                   11.5009(7)
_cell_length_c                   15.3888(8)
_cell_measurement_reflns_used    5090
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      61.5090
_cell_measurement_theta_min      3.9430
_cell_volume                     1831.24(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6144
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -26.00  74.00   1.00    1.00    --    0.00  77.00-120.00  100
  2  \w     58.00 151.00   1.00    1.00    --   82.59  30.00-120.00   93
  3  \w    117.00 147.00   1.00    1.00    --   82.59 125.00   0.00   30
  4  \w     26.00 105.00   1.00    1.00    --   82.59 -30.00  30.00   79
  5  \w     14.00 108.00   1.00    1.00    --   82.59 -94.00  60.00   94
  6  \w      4.00 102.00   1.00    1.00    --   82.59 -94.00 -60.00   98
  7  \w      5.00 100.00   1.00    1.00    --   82.59 -94.00-180.00   95
  8  \w      6.00  94.00   1.00    1.00    --   82.59 -30.00 -90.00   88
  9  \w    -89.00 -35.00   1.00    1.00    --    0.00-178.00 -30.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0588424000
_diffrn_orient_matrix_UB_12      0.0222541000
_diffrn_orient_matrix_UB_13      -0.0964936000
_diffrn_orient_matrix_UB_21      -0.0292487000
_diffrn_orient_matrix_UB_22      -0.1353886000
_diffrn_orient_matrix_UB_23      -0.0330206000
_diffrn_orient_matrix_UB_31      -0.1329271000
_diffrn_orient_matrix_UB_32      -0.0141923000
_diffrn_orient_matrix_UB_33      0.0202859000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.824
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8296
_diffrn_reflns_point_group_measured_fraction_full 0.824
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         61.589
_diffrn_reflns_theta_min         2.983
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.673
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76197
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_recrystallization_method Ethylacetate/Hexane
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.858
_refine_diff_density_min         -0.324
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         5452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0897P)^2^+0.9336P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1500
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4589
_reflns_number_total             5452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc10085f4.cif
_cod_data_source_block           16tyk-rt02
_cod_depositor_comments          'Adding full bibliography for 7119438.cif.'
_cod_original_cell_volume        1831.25(17)
_cod_database_code               7119438
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         'C44 H30 O4'
_reflns_odcompleteness_completeness 94.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     62.05
_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
2.a Secondary CH2 refined with riding coordinates:
 C101(H10D,H10E)
2.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C15(H15), C16(H16), C17(H17), C22(H22), C23(H23),
 C25(H25), C26(H26), C27(H27), C33(H33), C34(H34), C35(H35), C36(H36), C40(H40),
  C41(H41), C42(H42), C43(H43), C52(H52), C53(H53), C55(H55), C56(H56),
 C57(H57), C62(H62), C63(H63), C65(H65), C66(H66), C67(H67)
2.c Idealised Me refined as rotating group:
 C100(H10A,H10B,H10C), C105(H10F,H10G,H10H)
;
_olex2_date_sample_data_collection 2016-04-13
_olex2_date_sample_submission    2016-04-03
_olex2_exptl_crystal_mounting_method 'mounted on a loop'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.166
_oxdiff_exptl_absorpt_empirical_full_min 0.773