Pyrene-Fused s-Indacene.
Melidonie, Jason; Liu, Junzhi; Fu, Yubin; Weigand, Jan J.; Berger, Reinhard; Feng, Xinliang; The Journal of organic chemistry 83 (2018) 6633–6639; doi:10.1021/acs.joc.8b00925

data_4035850
_publ_section_title
;
 Pyrene-Fused s-Indacene.
;
_journal_issue                   12
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6633
_journal_page_last               6639
_journal_paper_doi               10.1021/acs.joc.8b00925
_journal_volume                  83
_journal_year                    2018
_chemical_formula_moiety         'C66 H56, 0.68(C6 H14)'
_chemical_formula_sum            'C70.08 H65.5'
_chemical_formula_weight         907.63
_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   geom
_audit_creation_date             2017-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-12-10 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 90.669(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5895(4)
_cell_length_b                   11.2987(3)
_cell_length_c                   16.7039(5)
_cell_measurement_reflns_used    6166
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0590
_cell_measurement_theta_min      3.2610
_cell_volume                     2564.60(13)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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     -4.00  32.00   0.50    3.00    --  -38.50  57.00-150.00   72
  2  \w      7.00 119.00   0.50    3.00    --   42.75  19.00-180.00  224
  3  \w     79.00 133.00   0.50   12.00    --  111.00 -45.00-180.00  108
  4  \w     64.00  91.00   0.50   12.00    --  111.00 -94.00-150.00   54
  5  \w     45.00  72.00   0.50   12.00    --  111.00 -45.00-180.00   54
  6  \w     49.00  79.00   0.50   12.00    --  111.00 -45.00 -90.00   60
  7  \w    110.00 148.00   0.50   12.00    --  111.00  30.00   0.00   76
  8  \w     95.00 131.00   0.50   12.00    --  111.00 -45.00  90.00   72
  9  \w     90.00 173.00   0.50   12.00    --  111.00  15.00 150.00  166
 10  \w     88.00 178.00   0.50   12.00    --  111.00  61.00  30.00  180
 11  \w     95.00 178.00   0.50   12.00    --  111.00 125.00-150.00  166
 12  \w     72.00 121.00   0.50   12.00    --  111.00 -30.00  60.00   98
 13  \w     70.00 106.00   0.50   12.00    --  111.00 -94.00 120.00   72
 14  \w     52.00 108.00   0.50   12.00    --  111.00 -61.00  90.00  112
 15  \w     44.00  71.00   0.50   12.00    --  111.00 -30.00  60.00   54
 16  \w     23.00  77.00   0.50    3.00    --   42.75 -99.00-150.00  108
 17  \w   -106.00 -52.00   0.50    3.00    --  -38.50 -57.00  60.00  108
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1073562000
_diffrn_orient_matrix_UB_12      -0.0293515000
_diffrn_orient_matrix_UB_13      0.0229452000
_diffrn_orient_matrix_UB_21      0.0331810000
_diffrn_orient_matrix_UB_22      0.0370616000
_diffrn_orient_matrix_UB_23      -0.0842347000
_diffrn_orient_matrix_UB_31      0.0149562000
_diffrn_orient_matrix_UB_32      0.1279615000
_diffrn_orient_matrix_UB_33      0.0296419000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0209
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13364
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.084
_diffrn_reflns_theta_min         3.252
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.964
_exptl_absorpt_correction_T_min  0.764
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       plate
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.954
_exptl_crystal_size_mid          0.315
_exptl_crystal_size_min          0.083
_refine_diff_density_max         0.591
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         5054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0646
_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^)+(0.1320P)^2^+0.7524P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1893
_refine_ls_wR_factor_ref         0.2038
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4150
_reflns_number_total             5054
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b00925_si_003.cif
_cod_data_source_block           feng062
_cod_original_cell_volume        2564.61(14)
_cod_original_formula_sum        'C70.08 H65.50'
_cod_database_code               4035850
_chemical_oxdiff_formula         'C128 H104 '
_chemical_oxdiff_usercomment     J-tBu
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Others
 Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(C36)=
 Sof(H36A)=Sof(H36B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C8(H8), C10(H10), C12(H12), C13(H13), C19(H19),
 C23(H23), C25(H25)
3.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
;
_shelx_res_checksum              79415
_shelx_hkl_checksum              65410
_shelx_shelxl_version_number     2014/7
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.853
_oxdiff_exptl_absorpt_empirical_full_min 0.286