<i>sp</i>-9-[<i>o</i>-(β-Chloro-α,α-dimethylethyl)phenyl]fluorene: an Unanticipated Exclusive Product from the Reaction of <i>sp</i>-9-(<i>o</i>-<i>tert</i>-Butylphenyl)-9-fluorenol with Thionyl Chloride
Robinson, Paul D.; Hou, Yuqing; Meyers, Cal Y.; Acta Crystallographica Section C 54 (1998) 1173–1175; doi:10.1107/S0108270198002911

data_2007523
_publ_section_title
;
 <i>sp</i>-9-[<i>o</i>-(\b-Chloro-\a,\a-dimethylethyl)phenyl]fluorene:
 an Unanticipated Exclusive Product from the Reaction of
 <i>sp</i>-9-(<i>o</i>-<i>tert</i>-Butylphenyl)-9-fluorenol with
 Thionyl Chloride
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1173
_journal_page_last               1175
_journal_paper_doi               10.1107/S0108270198002911
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C23 H21 Cl1'
_chemical_formula_sum            'C23 H21 Cl'
_chemical_formula_weight         332.87
_chemical_melting_point          450.2(8)
_chemical_name_systematic
;
sp-9-[o-(\b-Chloro-\a,\a-dimethylethyl)phenyl]fluorene
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                104.542(19)
_cell_angle_beta                 96.133(17)
_cell_angle_gamma                86.504(18)
_cell_formula_units_Z            2
_cell_length_a                   9.0116(17)
_cell_length_b                   12.073(3)
_cell_length_c                   8.4305(18)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      12.7
_cell_volume                     882.2(3)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1996)
;
_computing_data_reduction
'PROCESS in TEXSAN (Molecular Structure Corporation, 1995)'
_computing_molecular_graphics    'ORTEP (Johnson, 1965) in TEXSAN'
_computing_publication_material  'TEXSAN, SHELXL97 and PLATON (Spek, 1990)'
_computing_structure_refinement  'LS in TEXSAN and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985) in TEXSAN'
_diffrn_ambient_temperature      296
_diffrn_measurement_device_type  'Rigaku AFC-5S'
_diffrn_measurement_method       '\w/2\q scans (rate 6\% min^-1^ in \w)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.026
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6224
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0.50
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.253
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.34
_refine_diff_density_max         0.154
_refine_diff_density_min         -0.195
_refine_ls_extinction_coef       0.030(3)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    'H atoms riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3112
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.069
_refine_ls_R_factor_gt           0.035
_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^)+(0.0363P)^2^+0.1931P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.094
_reflns_number_gt                2142
_reflns_number_total             3112
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fg1442.cif
_cod_data_source_block           fg1442
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '449.5-451.0' was changed to
'450.2(8)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '449.5-451.0' was changed to
'450.2(8)' - the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_formula_sum        'C23 H21 Cl1'
_cod_database_code               2007523