1-Carboxyfluorenone: an Intramolecularly Hydrogen-Bonded γ-Keto Acid
Coté, M. L.; Lalancette, R. A.; Thompson, H. W.; Acta Crystallographica Section C 52 (1996) 1535–1537; doi:10.1107/S0108270195016155

data_2004985
_publ_section_title
;
 1-Carboxyfluorenone: an Intramolecularly Hydrogen-Bonded \g-Keto Acid
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1535
_journal_page_last               1537
_journal_paper_doi               10.1107/S0108270195016155
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C14 H8 O3'
_chemical_formula_sum            'C14 H8 O3'
_chemical_formula_weight         224.2
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_cell_angle_alpha                90.
_cell_angle_beta                 91.28(1)
_cell_angle_gamma                90.
_cell_formula_units_Z            4
_cell_length_a                   3.809(1)
_cell_length_b                   19.911(2)
_cell_length_c                   13.206(2)
_cell_measurement_reflns_used    14
_cell_measurement_temperature    296(1)
_cell_measurement_theta_max      11.1
_cell_measurement_theta_min      5.4
_cell_volume                     1001.3(3)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  'SHELXTL/PC (Sheldrick, 1990b)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990a)'
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       2\q/\q
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.05
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2046
_diffrn_reflns_theta_max         25.0
_diffrn_standards_decay_%        1.35
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.979
_exptl_absorpt_correction_type   'face-indexed numerical'
_exptl_crystal_colour            'deep orange'
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_density_meas      1.484(1)
_exptl_crystal_density_method    'floatation in cyclohexane/CCl~4~'
_exptl_crystal_description       'flat plate'
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.168
_refine_diff_density_min         -0.147
_refine_ls_extinction_coef       0.0160(10)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   0.75
_refine_ls_goodness_of_fit_obs   1.02
_refine_ls_hydrogen_treatment
;
All non-carboxyl H atoms were placed in calculated positions and allowed
to refine as riding models.  The carboxyl H3B was found in an electron
density difference map; the positional parameters of H3B were refined,
but its temperature factor was held constant.
;
_refine_ls_number_parameters     159
_refine_ls_number_reflns         1766
_refine_ls_R_factor_all          0.129
_refine_ls_R_factor_obs          0.047
_refine_ls_shift/esd_max         0.277
_refine_ls_shift/esd_mean        0.031
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.0371P)^2^]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.117
_refine_ls_wR_factor_obs         0.091
_reflns_number_observed          736
_reflns_number_total             1767
_reflns_observed_criterion       F>4\s(F)
_cod_data_source_file            fg1139.cif
_cod_data_source_block           lalancette
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2004985