#------------------------------------------------------------------------------
#$Date: 2017-10-13 08:28:26 +0300 (Fri, 13 Oct 2017) $
#$Revision: 201972 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/10/29/2102972.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2102972
loop_
_publ_author_name
'Turowska-Tyrk, Ilona'
'Bakowicz, Julia'
'Scheffer, John R.'
_publ_section_title
;
 Monitoring structural transformations in crystals. 11. Yang
 photocyclizations -- one type of reaction, but diversity of structural
 changes
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              933
_journal_page_last               940
_journal_paper_doi               10.1107/S0108768107051336
_journal_volume                  63
_journal_year                    2007
_chemical_formula_sum            'C24 H31 N O3'
_chemical_formula_weight         381.50
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   geom
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.8834(7)
_cell_length_b                   12.0641(15)
_cell_length_c                   25.924(3)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      3
_cell_volume                     2152.8(4)
_computing_cell_refinement       'CRYSALIS (Oxford Diffraction, 2003)'
_computing_data_collection       'CRYSALIS (Oxford Diffraction, 2003)'
_computing_data_reduction        'CRYSALIS (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SXELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Kuma KM4CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_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  0.0962
_diffrn_reflns_av_sigmaI/netI    0.1319
_diffrn_reflns_limit_h_max       3
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11650
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.06
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.9700
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.161
_refine_diff_density_min         -0.181
_refine_ls_abs_structure_details
;
 The absolute structure was assigned on the basis of known
 absolute configuration of the cation.
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.838
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.1848
_refine_ls_R_factor_gt           0.0609
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0813P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1379
_refine_ls_wR_factor_ref         0.1808
_reflns_number_gt                1344
_reflns_number_total             3741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bk5065.cif
_cod_data_source_block           100P
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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 'Orthorhombic' changed to
'orthorhombic' 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 
;
_cod_database_code               2102972
_cod_database_fobs_code          2102972
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1P 1.2109(11) -0.2905(7) 0.2299(4) 0.171(4) Uani d . 1
H H1AP 1.2248 -0.2141 0.2409 0.205 Uiso calc R 1
H H1BP 1.3370 -0.3251 0.2255 0.205 Uiso calc R 1
C C2P 1.0690(12) -0.3590(8) 0.2639(3) 0.165(4) Uani d . 1
H H2AP 1.1067 -0.4358 0.2687 0.198 Uiso calc R 1
H H2BP 1.0355 -0.3241 0.2965 0.198 Uiso calc R 1
C C3P 0.9215(9) -0.3403(5) 0.2210(2) 0.0838(18) Uani d . 1
C C4P 1.0791(9) -0.3044(5) 0.1838(2) 0.0834(17) Uani d . 1
C C5P 1.0461(8) -0.1992(4) 0.1517(2) 0.0738(15) Uani d . 1
C C6P 1.1927(7) -0.1550(5) 0.1222(2) 0.0849(17) Uani d . 1
H H6P 1.3132 -0.1898 0.1214 0.102 Uiso calc R 1
C C7P 1.1641(8) -0.0603(5) 0.0939(2) 0.0785(16) Uani d . 1
H H7P 1.2676 -0.0281 0.0764 0.094 Uiso calc R 1
C C8P 0.9815(7) -0.0126(4) 0.09136(18) 0.0554(13) Uani d . 1
C C9P 0.8368(7) -0.0592(4) 0.1197(2) 0.0702(15) Uani d . 1
H H9P 0.7128 -0.0290 0.1174 0.084 Uiso calc R 1
C C10P 0.8654(7) -0.1490(5) 0.1514(2) 0.0697(15) Uani d . 1
C C11P 0.7041(8) -0.1936(5) 0.1839(2) 0.101(2) Uani d . 1
H H11A 0.6317 -0.2487 0.1646 0.121 Uiso calc R 1
H H11B 0.6158 -0.1340 0.1930 0.121 Uiso calc R 1
C C12P 0.7855(10) -0.2452(7) 0.2322(3) 0.123(2) Uani d . 1
H H12A 0.6791 -0.2717 0.2534 0.148 Uiso calc R 1
H H12B 0.8547 -0.1890 0.2517 0.148 Uiso calc R 1
C C13P 0.8085(12) -0.4452(7) 0.2067(3) 0.143(3) Uani d . 1
H H13A 0.9000 -0.5029 0.1973 0.171 Uiso calc R 1
H H13B 0.7283 -0.4298 0.1768 0.171 Uiso calc R 1
C C14P 0.6759(13) -0.4887(6) 0.2513(4) 0.193(5) Uani d . 1
H H14A 0.6068 -0.5533 0.2399 0.290 Uiso calc R 1
H H14B 0.5848 -0.4321 0.2609 0.290 Uiso calc R 1
H H14C 0.7549 -0.5075 0.2806 0.290 Uiso calc R 1
C C15P 0.9436(9) 0.0889(4) 0.0589(2) 0.0702(15) Uani d . 1
O O1P 1.0846(5) 0.1502(3) 0.04827(15) 0.0852(11) Uani d . 1
O O2P 0.7763(5) 0.1053(3) 0.04271(16) 0.0926(13) Uani d . 1
O O3P 1.1520(7) -0.3910(4) 0.1523(2) 0.145(2) Uani d . 1
C C16P 0.4649(9) 0.3204(5) 0.0902(3) 0.0898(18) Uani d . 1
H H16P 0.3366 0.3547 0.0939 0.108 Uiso calc R 1
C C17P 0.5053(11) 0.2554(6) 0.1386(2) 0.141(3) Uani d . 1
H H17A 0.4051 0.2010 0.1435 0.211 Uiso calc R 1
H H17B 0.5079 0.3048 0.1676 0.211 Uiso calc R 1
H H17C 0.6287 0.2188 0.1355 0.211 Uiso calc R 1
C C18P 0.6063(7) 0.4101(6) 0.0774(2) 0.0723(15) Uani d . 1
C C19P 0.7972(8) 0.3877(5) 0.0682(2) 0.0826(17) Uani d . 1
H H19P 0.8435 0.3163 0.0738 0.099 Uiso calc R 1
C C20P 0.9234(8) 0.4680(6) 0.0511(2) 0.0913(18) Uani d . 1
H H20P 1.0518 0.4493 0.0441 0.110 Uiso calc R 1
C C21P 0.8624(11) 0.5760(6) 0.0439(2) 0.0882(17) Uani d . 1
C C22P 0.6748(11) 0.5999(5) 0.0573(3) 0.106(2) Uani d . 1
H H22P 0.6310 0.6727 0.0556 0.127 Uiso calc R 1
C C23P 0.5500(9) 0.5177(7) 0.0733(2) 0.0956(19) Uani d . 1
H H23P 0.4227 0.5364 0.0817 0.115 Uiso calc R 1
C C24P 0.9957(11) 0.6625(6) 0.0212(3) 0.145(3) Uani d . 1
H H24A 0.9850 0.6614 -0.0157 0.217 Uiso calc R 1
H H24B 1.1273 0.6466 0.0310 0.217 Uiso calc R 1
H H24C 0.9595 0.7343 0.0339 0.217 Uiso calc R 1
N N1P 0.4542(5) 0.2414(4) 0.04694(17) 0.0790(14) Uani d . 1
H H1CP 0.3695 0.1880 0.0545 0.118 Uiso calc R 1
H H1DP 0.5708 0.2117 0.0416 0.118 Uiso calc R 1
H H1EP 0.4158 0.2767 0.0186 0.118 Uiso calc R 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C4P C1P C2P 90.7(6)
C3P C2P C1P 85.7(5)
C12P C3P C4P 110.5(5)
C12P C3P C2P 112.6(7)
C4P C3P C2P 91.7(5)
C12P C3P C13P 111.1(6)
C4P C3P C13P 116.5(6)
C2P C3P C13P 113.2(6)
O3P C4P C1P 109.0(6)
O3P C4P C3P 114.2(5)
C1P C4P C3P 87.6(5)
O3P C4P C5P 110.5(5)
C1P C4P C5P 115.2(6)
C3P C4P C5P 118.4(5)
C6P C5P C10P 119.2(5)
C6P C5P C4P 120.9(5)
C10P C5P C4P 119.9(5)
C7P C6P C5P 121.0(5)
C6P C7P C8P 120.2(5)
C9P C8P C7P 117.9(4)
C9P C8P C15P 120.7(4)
C7P C8P C15P 121.5(5)
C8P C9P C10P 123.0(5)
C9P C10P C5P 118.5(5)
C9P C10P C11P 121.0(5)
C5P C10P C11P 120.5(5)
C10P C11P C12P 109.9(5)
C11P C12P C3P 112.6(6)
C3P C13P C14P 113.3(7)
O2P C15P O1P 123.4(5)
O2P C15P C8P 118.6(5)
O1P C15P C8P 118.0(5)
N1P C16P C18P 109.4(5)
N1P C16P C17P 107.8(5)
C18P C16P C17P 116.3(5)
C23P C18P C19P 116.8(6)
C23P C18P C16P 121.6(5)
C19P C18P C16P 121.6(6)
C18P C19P C20P 121.7(6)
C19P C20P C21P 121.1(5)
C22P C21P C20P 116.8(6)
C22P C21P C24P 121.9(7)
C20P C21P C24P 121.3(7)
C21P C22P C23P 121.0(6)
C18P C23P C22P 122.2(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1P C4P 1.509(9)
C1P C2P 1.555(9)
C2P C3P 1.524(8)
C3P C12P 1.510(8)
C3P C4P 1.514(7)
C3P C13P 1.530(9)
C4P O3P 1.418(6)
C4P C5P 1.535(7)
C5P C6P 1.374(7)
C5P C10P 1.383(6)
C6P C7P 1.372(7)
C7P C8P 1.384(6)
C8P C9P 1.359(6)
C8P C15P 1.508(7)
C9P C10P 1.375(7)
C10P C11P 1.494(7)
C11P C12P 1.507(8)
C13P C14P 1.564(9)
C15P O2P 1.242(6)
C15P O1P 1.251(6)
C16P N1P 1.473(7)
C16P C18P 1.493(7)
C16P C17P 1.506(8)
C18P C23P 1.359(7)
C18P C19P 1.363(6)
C19P C20P 1.375(7)
C20P C21P 1.382(7)
C21P C22P 1.368(8)
C21P C24P 1.508(8)
C22P C23P 1.376(8)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30654488
