A new polymorph and two inclusion compounds of 9,9'-spirobifluorene
Douthwaite, Richard E.; Taylor, Andrew; Whitwood, Adrian C.; Acta Crystallographica Section C 61 (2005) o328–o331; doi:10.1107/S0108270105009479

data_2014843
_publ_section_title
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 A new polymorph and two inclusion compounds of 9,9'-spirobifluorene
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_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o328
_journal_page_last               o331
_journal_paper_doi               10.1107/S0108270105009479
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C25 H16 , C12 H10'
_chemical_formula_moiety         'C25 H16 , C12 H10'
_chemical_formula_sum            'C37 H26'
_chemical_formula_weight         470.58
_chemical_name_systematic
;
9,9'-spirobifluorene--biphenyl (1/1)
;
_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           SHELXL97
_cell_angle_alpha                71.339(8)
_cell_angle_beta                 83.106(9)
_cell_angle_gamma                67.030(7)
_cell_formula_units_Z            2
_cell_length_a                   9.774(4)
_cell_length_b                   11.427(4)
_cell_length_c                   13.075(5)
_cell_measurement_reflns_used    944
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      24.24
_cell_measurement_theta_min      2.41
_cell_volume                     1273.8(8)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        SAINT-Plus
_computing_molecular_graphics    'CAMERON (Watkin <i>et al.</i>, 1996)'
_computing_publication_material  'SHELXTL (Bruker, 2001)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      115(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0495
_diffrn_reflns_av_sigmaI/netI    0.2347
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6971
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
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_refine_ls_extinction_coef       0.022(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'Please provide'
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_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.0785
_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^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1874
_refine_ls_wR_factor_ref         0.2480
_reflns_number_gt                2416
_reflns_number_total             4476
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gg1249.cif
_cod_data_source_block           II
_cod_depositor_comments
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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 1527 2010-12-29 10:47:43Z saulius 

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_values 1715 2011-07-08 13:25:40Z adriana 

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 
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_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2014843