The surprising <i>sp</i> rotameric structure of 9-methyl-9-pivaloylfluorene
Meyers, Cal Y.; Lutfi, Hisham G.; Varol, Pninit; Hou, Yuqing; Robinson, Paul D.; Acta Crystallographica Section C 56 (2000) 1468–1470; doi:10.1107/S010827010001235X

data_2011607
_publ_section_title
;
 The surprising <i>sp</i> rotameric structure of
 9-methyl-9-pivaloylfluorene
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1468
_journal_page_last               1470
_journal_paper_doi               10.1107/S010827010001235X
_journal_volume                  56
_journal_year                    2000
_chemical_formula_moiety         ' C19 H20 O1'
_chemical_formula_sum            'C19 H20 O'
_chemical_formula_weight         264.35
_chemical_melting_point          431.0(5)
_chemical_name_systematic
;
sp-9-methyl-9-pivaloylfluorene
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.908(2)
_cell_length_b                   15.3513(18)
_cell_length_c                   7.1860(6)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296
_cell_measurement_theta_max      10.5
_cell_measurement_theta_min      10.0
_cell_volume                     1534.3(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, 1997)
;
_computing_molecular_graphics    'ORTEP (Johnson, 1965)'
_computing_publication_material
;
TEXSAN, SHELXL97 and PLATON (Spek, 2000)
;
_computing_structure_refinement  'TEXSAN and SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku AFC-5S'
_diffrn_measurement_method       '\w (rate 6\% min^-1^)'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71069
_diffrn_reflns_av_R_equivalents  .023
_diffrn_reflns_av_sigmaI/netI    .0362
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1137
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        .7
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    .069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_density_meas      ?
_exptl_crystal_description       fragment
_exptl_crystal_F_000             568
_exptl_crystal_size_max          .51
_exptl_crystal_size_mid          .49
_exptl_crystal_size_min          .43
_refine_diff_density_max         .26
_refine_diff_density_min         -.13
_refine_ls_abs_structure_details
;
Absolute structure could not be determined
;
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_coef       .025(4)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         997
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          .072
_refine_ls_R_factor_gt           .043
_refine_ls_shift/su_max          .001
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0884P)^2^+0.0776P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .138
_reflns_number_gt                691
_reflns_number_total             997
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd1104.cif
_cod_data_source_block           III
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '430.5-431.5' was changed to
'431.0(5)' - 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 '430.5-431.5' was changed to
'431.0(5)' - the average value was taken and precision was estimated.

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 
;
_cod_database_code               2011607
_cod_database_fobs_code          2011607