Correlation of Structure with Crystalline to Amorphous Phase Transitions of 1,3,6-Substituted Fulvene Derived Molecular Glasses.
Brown, Loren C.; Peloquin, Andrew; Godman, Nicholas P.; Balaich, Gary James; Iacono, Scott T.; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c01014

data_4038626
_publ_section_title
;
 Correlation of Structure with Crystalline to Amorphous Phase Transitions
 of 1,3,6-Substituted Fulvene Derived Molecular Glasses.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01014
_journal_year                    2020
_chemical_formula_moiety         'C30 H22'
_chemical_formula_sum            'C30 H22'
_chemical_formula_weight         382.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_cell_length_a                   11.7922(2)
_cell_length_b                   7.31440(10)
_cell_length_c                   23.5196(3)
_cell_measurement_reflns_used    9754
_cell_measurement_temperature    100
_cell_measurement_theta_max      68.28
_cell_measurement_theta_min      3.75
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_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 v2017.3-0 (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
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_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_av_unetI/netI     0.0133
_diffrn_reflns_Laue_measured_fraction_full 0.976
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_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48662
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.500
_diffrn_reflns_theta_max         71.217
_diffrn_reflns_theta_min         1.879
_diffrn_source                   'Micro Focus Rotating Anode'
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_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0710 before and 0.0327 after correction.
The Ratio of minimum to maximum transmission is 0.9023.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.224
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.028
_refine_ls_abs_structure_details
;
 Flack x determined using 3408 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.28(14)
_refine_ls_extinction_coef       0.0016(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         7551
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0256
_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^)+(0.0376P)^2^+0.3602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0692
_refine_ls_wR_factor_ref         0.0693
_reflns_Friedel_coverage         0.839
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                7507
_reflns_number_total             7551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01014_si_003.cif
_cod_data_source_block           balaich01
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/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 7556 2019-12-06 15:28:31Z antanas 
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_cod_database_code               4038626
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_shelx_estimated_absorpt_t_max   0.969
_shelx_estimated_absorpt_t_min   0.924
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C2'(H2'),
 C4'(H4'), C6'(H6'), C8'(H8'), C9'(H9'), C10'(H10'), C11'(H11'), C12'(H12'),
 C14'(H14'), C15'(H15'), C16'(H16'), C17'(H17'), C18'(H18'), C20'(H20'),
 C21'(H21'), C23'(H23'), C24'(H24'), C26'(H26'), C27'(H27'), C28'(H28'),
 C29'(H29'), C30'(H30')
;
_shelx_res_checksum              86695
_shelx_hkl_checksum              42877
_olex2_submission_special_instructions 'No special instructions were received'