1-<i>tert</i>-Butyl-9-methoxy-4-methyl-1,2,3,4-tetrahydro-2-azafluoren-3-one, a Novel Fluorenone
García-Granda, Santiago; Santiago-García, Rafael; Sanni, S. Bamidele; Suárez-Sobrino, Angel; Santamaría, Javier; Acta Crystallographica Section C 54 (1998) 1961–1963; doi:10.1107/S0108270198008257

data_2007910
_publ_section_title
;1-<i>tert</i>-Butyl-9-methoxy-4-methyl-1,2,3,4-tetrahydro-2-azafluoren-3-one,
 a Novel Fluorenone
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1961
_journal_page_last               1963
_journal_paper_doi               10.1107/S0108270198008257
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C18 H23 N1 O2'
_chemical_formula_sum            'C18 H23 N O2'
_chemical_formula_weight         285.37
_chemical_name_systematic
;
 2-aza-1-tertbuthyl-4-methyl-9-methoxy-1,2,3,4-tetrahydro-fluoren-2-one.
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.37(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.571(3)
_cell_length_b                   6.3565(15)
_cell_length_c                   24.360(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      13
_cell_volume                     1610.1(9)
_computing_cell_refinement       'CRYSDA (Beurskens et al., 1992)'
_computing_data_collection
;CAD-4 Software (Enraf-Nonius, 1989), with profile analysis over all
 reflections
(Lehmann & Larsen, 1974; Grant & Gabe, 1978)
;
_computing_data_reduction
'THE REFLEX (Garc\'ia-Granda, Aguirre-P\'erez et al., 1997)'
_computing_molecular_graphics    'EUCLID (Spek, 1982)'
_computing_publication_material
;
SHELXL97. Geometrical calculations: PARST (Nardelli, 1983).
All calculations were made at the University of Oviedo on the Scientific
Computer Center and X-Ray group VAX/AXP computers
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.909
_diffrn_measured_fraction_theta_max 0.909
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w-2\Q
_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  0.085
_diffrn_reflns_av_sigmaI/netI    0.1087
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            6400
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        5.32
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   'refined from \DF (Parkin et al., 1995)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.190
_refine_diff_density_min         -0.193
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.979
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     282
_refine_ls_number_reflns         2836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.172
_refine_ls_R_factor_gt           0.048
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0619P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.145
_reflns_number_gt                1163
_reflns_number_total             2836
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            da1018.cif
_cod_data_source_block           js882
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 'Monoclinic' changed to 'monoclinic'
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:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0619P)^2^] where P = (Fo^2^+2Fc^2^)/3' was changed
to 'calc'. New tag '_refine_ls_weighting_details' was created. The
value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0619P)^2^]
where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1610.2(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C18 H23 N1 O2'
_cod_database_code               2007910