#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/02/41/4024141.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4024141
loop_
_publ_author_name
'Hideko Koshima'
'Michitaro Fukano'
'Hidehiro Uekusa'
_publ_section_title
;
 Diastereospecific Photocyclization of a Isopropylbenzophenone
 Derivative in Crystals and the Morphological Changes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6786
_journal_page_last               6791
_journal_paper_doi               10.1021/jo071005i
_journal_volume                  72
_journal_year                    2007
_chemical_formula_moiety         'C31 H37 N O2 '
_chemical_formula_sum            'C31 H37 N O2'
_chemical_formula_weight         455.64
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      76
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.1250(8)
_cell_length_b                   11.1250(8)
_cell_length_c                   22.9386(19)
_cell_measurement_reflns_used    22314
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      68.0
_cell_measurement_theta_min      3.9
_cell_volume                     2839.0(4)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  SHELXL
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       w
_diffrn_radiation_type           'Cu K'a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            28913
_diffrn_reflns_theta_full        68.03
_diffrn_reflns_theta_max         68.03
_exptl_absorpt_coefficient_mu    0.507
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984.00
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.21
_refine_diff_density_min         -0.17
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  2249 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_coef       0.0023(4)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.268
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4919
_refine_ls_R_factor_gt           0.0625
_refine_ls_shift/su_max          0.2940
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/['s²(Fo²)+(0.1000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1890
_reflns_number_gt                3601
_reflns_number_total             4919
_reflns_threshold_expression     F²>2.0's(F²)
_cod_data_source_file            jo071005i-File001_3.cif
_cod_data_source_block           '_fukano10-2-S,S-2'
_cod_original_formula_sum        'C31 H37 N O2 '
_cod_database_code               4024141
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -Y,+X,1/4+Z
3 -X,-Y,1/2+Z
4 +Y,-X,3/4+Z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O(1) O 0.4737(2) 0.25530(19) 0.75125(9) 0.0702(6) Uani 1.00 1 d . . .
O(2) O 0.3350(2) 0.4336(2) 0.72187(11) 0.0875(7) Uani 1.00 1 d . . .
N(1) N 0.2842(2) 0.5134(2) 0.63510(12) 0.0699(7) Uani 1.00 1 d . . .
C(1) C 0.3270(2) 0.3028(2) 0.63866(12) 0.0609(7) Uani 1.00 1 d . . .
C(4) C 0.4233(2) 0.2204(2) 0.64923(12) 0.0567(7) Uani 1.00 1 d . . .
C(6) C 0.6295(2) 0.1585(2) 0.69334(14) 0.0627(7) Uani 1.00 1 d . . .
C(7) C 0.5221(2) 0.2441(2) 0.69386(13) 0.0593(7) Uani 1.00 1 d . . .
C(8) C 0.2438(3) 0.1677(3) 0.56635(17) 0.0748(9) Uani 1.00 1 d . . .
C(9) C 0.4274(2) 0.1177(3) 0.61596(16) 0.0693(8) Uani 1.00 1 d . . .
C(10) C 0.2409(2) 0.2721(3) 0.59740(16) 0.0698(8) Uani 1.00 1 d . . .
C(11) C 0.3155(2) 0.4193(3) 0.66888(16) 0.0676(8) Uani 1.00 1 d . . .
C(12) C 0.8273(3) 0.2227(3) 0.66456(16) 0.0730(8) Uani 1.00 1 d . . .
C(13) C 0.3393(3) 0.0894(3) 0.57480(18) 0.0794(10) Uani 1.00 1 d . . .
C(14) C 0.7082(2) 0.2454(2) 0.67529(14) 0.0648(7) Uani 1.00 1 d . . .
C(15) C 0.6637(3) 0.0404(2) 0.70383(16) 0.0702(8) Uani 1.00 1 d . . .
C(16) C 0.7861(3) 0.0201(3) 0.69285(17) 0.0782(9) Uani 1.00 1 d . . .
C(17) C 0.6177(2) 0.3475(2) 0.67506(14) 0.0644(8) Uani 1.00 1 d . . .
C(18) C 0.8669(3) 0.1059(3) 0.67335(17) 0.0768(9) Uani 1.00 1 d . . .
C(19) C 0.2725(3) 0.6355(2) 0.66090(17) 0.0754(9) Uani 1.00 1 d . . .
C(20) C 0.6383(3) 0.4425(3) 0.72182(19) 0.0868(11) Uani 1.00 1 d . . .
C(21) C 0.5786(4) -0.0541(3) 0.7253(2) 0.0924(11) Uani 1.00 1 d . . .
C(22) C 0.5999(3) 0.4036(3) 0.61522(19) 0.0868(11) Uani 1.00 1 d . . .
C(23) C 0.1577(4) 0.6483(3) 0.6952(2) 0.0953(12) Uani 1.00 1 d . . .
C(24) C 0.2842(3) 0.7266(3) 0.6118(2) 0.0915(11) Uani 1.00 1 d . . .
C(25) C 1.0004(3) 0.0763(4) 0.6623(2) 0.1073(15) Uani 1.00 1 d . . .
C(26) C 0.0472(18) 0.7082(13) 0.7825(5) 0.270(11) Uani 1.00 1 d . . .
C(27) C 0.1596(8) 0.6894(6) 0.7498(2) 0.172(3) Uani 1.00 1 d . . .
C(28) C -0.048(2) 0.6756(12) 0.7536(8) 0.286(14) Uani 1.00 1 d . . .
C(29) C 0.0478(5) 0.6223(5) 0.6678(4) 0.164(3) Uani 1.00 1 d . . .
C(30) C 1.0174(6) -0.0358(6) 0.6320(4) 0.179(3) Uani 1.00 1 d . . .
C(31) C 1.0753(4) 0.0965(9) 0.7121(3) 0.184(3) Uani 1.00 1 d . . .
C(32) C 0.5896(6) -0.1723(4) 0.6932(4) 0.163(2) Uani 1.00 1 d . . .
C(33) C 0.5858(11) -0.0698(8) 0.7867(3) 0.241(6) Uani 1.00 1 d . . .
C(34) C -0.0626(7) 0.6392(7) 0.6968(8) 0.224(5) Uani 1.00 1 d . . .
H(1) H 0.4143 0.3244 0.7506 0.068 Uiso 1.00 1 c R . .
H(2) H 0.2823 0.4979 0.5884 0.068 Uiso 1.00 1 c R . .
H(3) H 0.1830 0.1493 0.5400 0.090 Uiso 1.00 1 c R . .
H(4) H 0.4914 0.0650 0.6211 0.083 Uiso 1.00 1 c R . .
H(5) H 0.1780 0.3254 0.5907 0.084 Uiso 1.00 1 c R . .
H(6) H 0.8792 0.2829 0.6520 0.088 Uiso 1.00 1 c R . .
H(7) H 0.3446 0.0188 0.5533 0.095 Uiso 1.00 1 c R . .
H(8) H 0.8153 -0.0571 0.6992 0.094 Uiso 1.00 1 c R . .
H(9) H 0.3400 0.6476 0.6877 0.090 Uiso 1.00 1 c R . .
H(10) H 0.5824 0.5073 0.7165 0.104 Uiso 1.00 1 c R . .
H(11) H 0.7189 0.4726 0.7189 0.104 Uiso 1.00 1 c R . .
H(12) H 0.6265 0.4073 0.7596 0.104 Uiso 1.00 1 c R . .
H(13) H 0.4975 -0.0240 0.7173 0.111 Uiso 1.00 1 c R . .
H(14) H 0.6432 0.3578 0.5867 0.104 Uiso 1.00 1 c R . .
H(15) H 0.6293 0.4847 0.6156 0.104 Uiso 1.00 1 c R . .
H(16) H 0.5159 0.4036 0.6057 0.104 Uiso 1.00 1 c R . .
H(17) H 0.3672 0.7475 0.6067 0.110 Uiso 1.00 1 c R . .
H(18) H 0.2390 0.7974 0.6213 0.110 Uiso 1.00 1 c R . .
H(19) H 0.2537 0.6924 0.5763 0.110 Uiso 1.00 1 c R . .
H(20) H 1.0263 0.1373 0.6342 0.129 Uiso 1.00 1 c R . .
H(21) H 0.0446 0.7401 0.8199 0.324 Uiso 1.00 1 c R . .
H(22) H 0.2329 0.7064 0.7675 0.207 Uiso 1.00 1 c R . .
H(23) H -0.1192 0.6774 0.7752 0.343 Uiso 1.00 1 c R . .
H(24) H 0.0478 0.5935 0.6297 0.197 Uiso 1.00 1 c R . .
H(25) H 1.0276 -0.0994 0.6599 0.214 Uiso 1.00 1 c R . .
H(26) H 1.0876 -0.0306 0.6078 0.214 Uiso 1.00 1 c R . .
H(27) H 0.9483 -0.0522 0.6082 0.214 Uiso 1.00 1 c R . .
H(28) H 1.1019 0.1786 0.7124 0.221 Uiso 1.00 1 c R . .
H(29) H 1.1438 0.0442 0.7104 0.221 Uiso 1.00 1 c R . .
H(30) H 1.0305 0.0803 0.7470 0.221 Uiso 1.00 1 c R . .
H(31) H 0.5362 -0.1724 0.6603 0.195 Uiso 1.00 1 c R . .
H(32) H 0.5688 -0.2371 0.7190 0.195 Uiso 1.00 1 c R . .
H(33) H 0.6708 -0.1824 0.6799 0.195 Uiso 1.00 1 c R . .
H(34) H 0.6449 -0.1301 0.7955 0.289 Uiso 1.00 1 c R . .
H(35) H 0.5090 -0.0949 0.8014 0.289 Uiso 1.00 1 c R . .
H(36) H 0.6085 0.0047 0.8046 0.289 Uiso 1.00 1 c R . .
H(37) H -0.1371 0.6269 0.6794 0.269 Uiso 1.00 1 c R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.018 0.009
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.049 0.032
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.031 0.018
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
