#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/02/41/4024140.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_4024140
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           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90.0000
_cell_angle_beta                 97.056(8)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   10.1187(15)
_cell_length_b                   9.4944(14)
_cell_length_c                   14.032(2)
_cell_measurement_reflns_used    12203
_cell_measurement_temperature    296.1
_cell_measurement_theta_max      68.2
_cell_measurement_theta_min      3.2
_cell_volume                     1337.8(3)
_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 0.967
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID'
_diffrn_measurement_method       w
_diffrn_radiation_type           'Cu K'a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13272
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_exptl_absorpt_coefficient_mu    0.538
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.716
_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    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             492.00
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.20
_refine_diff_density_min         -0.23
_refine_ls_abs_structure_details
'Flack, H. D. (1983), Acta Cryst. A39, 876-881.  1962 Friedel Pairs'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_coef       0.0070(11)
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.258
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     309
_refine_ls_number_reflns         4487
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.0020
_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         0.1711
_reflns_number_gt                3617
_reflns_number_total             4487
_reflns_threshold_expression     F²>2.0's(F²)
_cod_data_source_file            jo071005i-File001_2.cif
_cod_data_source_block           '_fukano06-R,S-2'
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C31 H37 N O2 '
_cod_database_code               4024140
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,-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 -1.1974(2) -0.3813(2) -0.71619(13) 0.0717(5) Uani 1.00 1 d . . .
O(2) O -1.0990(2) -0.3859(2) -0.53083(13) 0.0720(5) Uani 1.00 1 d . . .
N(3) N -1.0454(2) -0.1833(2) -0.45322(14) 0.0575(5) Uani 1.00 1 d . . .
C(4) C -1.0425(2) -0.2701(2) -0.52663(18) 0.0532(6) Uani 1.00 1 d . . .
C(5) C -0.9618(2) -0.2220(2) -0.60308(18) 0.0506(5) Uani 1.00 1 d . . .
C(6) C -1.0092(2) -0.2193(3) -0.70162(18) 0.0552(6) Uani 1.00 1 d . . .
C(7) C -0.8317(2) -0.1855(3) -0.5723(2) 0.0607(6) Uani 1.00 1 d . . .
C(8) C -1.2580(2) -0.1706(3) -0.38406(19) 0.0607(6) Uani 1.00 1 d . . .
C(9) C -1.1954(2) -0.2205(3) -0.84722(19) 0.0648(7) Uani 1.00 1 d . . .
C(10) C -1.1536(2) -0.2467(2) -0.74066(18) 0.0586(6) Uani 1.00 1 d . . .
C(11) C -1.2789(2) -0.1115(3) -0.8322(2) 0.0670(7) Uani 1.00 1 d . . .
C(12) C -1.2907(3) -0.0321(3) -0.3941(2) 0.0804(9) Uani 1.00 1 d . . .
C(13) C -1.1148(2) -0.2188(3) -0.36977(18) 0.0625(7) Uani 1.00 1 d . . .
C(14) C -0.7896(2) -0.1435(3) -0.7314(2) 0.0744(8) Uani 1.00 1 d . . .
C(15) C -1.2544(2) -0.1175(3) -0.7234(2) 0.0659(7) Uani 1.00 1 d . . .
C(16) C -0.9205(2) -0.1766(3) -0.7634(2) 0.0698(7) Uani 1.00 1 d . . .
C(17) C -0.7453(2) -0.1477(3) -0.6368(2) 0.0654(7) Uani 1.00 1 d . . .
C(18) C -1.0376(3) -0.1549(4) -0.2803(2) 0.0800(9) Uani 1.00 1 d . . .
C(19) C -1.1791(3) -0.2729(4) -0.9372(2) 0.0769(8) Uani 1.00 1 d . . .
C(20) C -1.3611(3) -0.2642(4) -0.3894(2) 0.0914(10) Uani 1.00 1 d . . .
C(21) C -1.1918(3) 0.0161(3) -0.6784(2) 0.0792(9) Uani 1.00 1 d . . .
C(22) C -1.3424(3) -0.0901(4) -0.9989(2) 0.0886(10) Uani 1.00 1 d . . .
C(23) C -1.3732(2) -0.1605(4) -0.6762(2) 0.0862(10) Uani 1.00 1 d . . .
C(24) C -1.2581(4) -0.1994(4) -1.0120(2) 0.0918(11) Uani 1.00 1 d . . .
C(25) C -1.0971(4) -0.3999(4) -0.9521(2) 0.0952(11) Uani 1.00 1 d . . .
C(26) C -1.3543(3) -0.0426(4) -0.9070(2) 0.0873(9) Uani 1.00 1 d . . .
C(27) C -1.5194(3) -0.0805(4) -0.4076(3) 0.0958(11) Uani 1.00 1 d . . .
C(28) C -1.4206(3) 0.0118(4) -0.4052(3) 0.0935(11) Uani 1.00 1 d . . .
C(29) C -1.4920(3) -0.2189(5) -0.4024(3) 0.1067(13) Uani 1.00 1 d . . .
C(30) C -1.4194(5) -0.0179(6) -1.0844(3) 0.1266(17) Uani 1.00 1 d . . .
C(31) C -1.0171(5) -0.3939(6) -1.0367(4) 0.1384(18) Uani 1.00 1 d . . .
C(32) C -1.5020(6) -0.1113(9) -1.1437(4) 0.173(2) Uani 1.00 1 d . . .
C(33) C -1.1779(7) -0.5314(6) -0.9581(5) 0.174(2) Uani 1.00 1 d . . .
C(34) C -1.3536(7) 0.1034(8) -1.1155(5) 0.194(3) Uani 1.00 1 d . . .
H(1) H -0.8015 -0.1864 -0.5070 0.073 Uiso 1.00 1 c R . .
H(2) H -1.2231 0.0345 -0.3933 0.096 Uiso 1.00 1 c R . .
H(3) H -1.1139 -0.3215 -0.3623 0.075 Uiso 1.00 1 c R . .
H(4) H -0.7318 -0.1182 -0.7752 0.089 Uiso 1.00 1 c R . .
H(5) H -0.9499 -0.1698 -0.8287 0.084 Uiso 1.00 1 c R . .
H(6) H -0.6573 -0.1253 -0.6151 0.078 Uiso 1.00 1 c R . .
H(7) H -1.0708 -0.0620 -0.2704 0.096 Uiso 1.00 1 c R . .
H(8) H -0.9449 -0.1495 -0.2884 0.096 Uiso 1.00 1 c R . .
H(9) H -1.0484 -0.2127 -0.2257 0.096 Uiso 1.00 1 c R . .
H(10) H -1.3429 -0.3601 -0.3843 0.110 Uiso 1.00 1 c R . .
H(11) H -1.1695 0.0780 -0.7281 0.095 Uiso 1.00 1 c R . .
H(12) H -1.1126 -0.0075 -0.6366 0.095 Uiso 1.00 1 c R . .
H(13) H -1.2539 0.0621 -0.6422 0.095 Uiso 1.00 1 c R . .
H(14) H -1.3524 -0.1529 -0.6078 0.103 Uiso 1.00 1 c R . .
H(15) H -1.3962 -0.2562 -0.6930 0.103 Uiso 1.00 1 c R . .
H(16) H -1.4469 -0.1001 -0.6976 0.103 Uiso 1.00 1 c R . .
H(17) H -1.2520 -0.2278 -1.0747 0.110 Uiso 1.00 1 c R . .
H(18) H -1.0323 -0.4088 -0.8945 0.114 Uiso 1.00 1 c R . .
H(19) H -1.4102 0.0319 -0.8961 0.105 Uiso 1.00 1 c R . .
H(20) H -1.6072 -0.0495 -0.4129 0.115 Uiso 1.00 1 c R . .
H(21) H -1.4397 0.1075 -0.4111 0.112 Uiso 1.00 1 c R . .
H(22) H -1.5609 -0.2843 -0.4074 0.128 Uiso 1.00 1 c R . .
H(23) H -1.4876 0.0289 -1.0519 0.152 Uiso 1.00 1 c R . .
H(24) H -0.9324 -0.3505 -1.0169 0.166 Uiso 1.00 1 c R . .
H(25) H -1.0648 -0.3396 -1.0875 0.166 Uiso 1.00 1 c R . .
H(26) H -1.0035 -0.4877 -1.0591 0.166 Uiso 1.00 1 c R . .
H(27) H -1.5856 -0.1217 -1.1188 0.207 Uiso 1.00 1 c R . .
H(28) H -1.4593 -0.2014 -1.1449 0.207 Uiso 1.00 1 c R . .
H(29) H -1.5171 -0.0740 -1.2077 0.207 Uiso 1.00 1 c R . .
H(30) H -1.2135 -0.5484 -1.0237 0.208 Uiso 1.00 1 c R . .
H(31) H -1.2497 -0.5214 -0.9198 0.208 Uiso 1.00 1 c R . .
H(32) H -1.1227 -0.6092 -0.9347 0.208 Uiso 1.00 1 c R . .
H(33) H -1.3033 0.0777 -1.1665 0.233 Uiso 1.00 1 c R . .
H(34) H -1.2947 0.1409 -1.0627 0.233 Uiso 1.00 1 c R . .
H(35) H -1.4186 0.1733 -1.1381 0.233 Uiso 1.00 1 c R . .
H(36) H -1.1685 -0.4122 -0.6388 0.068 Uiso 1.00 1 c R . .
H(37) H -0.9943 -0.0939 -0.4523 0.068 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)
;
