#------------------------------------------------------------------------------
#$Date: 2021-10-06 16:44:14 +0300 (Wed, 06 Oct 2021) $
#$Revision: 269609 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/88/7128811.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_7128811
loop_
_publ_author_name
'Mondal, Atanu'
'Shivangi, ?'
'Tung, Pinku'
'Wagulde, Siddhant V.'
'Ramasastry, S. S. V.'
_publ_section_title
;
 Annulative Morita-Baylis-Hillman reaction to synthesise chiral
 dibenzocycloheptanes.
;
_journal_issue                   73
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9260
_journal_page_last               9263
_journal_paper_doi               10.1039/d1cc02765d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C26 H18 O2'
_chemical_formula_sum            'C26 H18 O2'
_chemical_formula_weight         362.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-17 deposited with the CCDC.	2021-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.527(16)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.3826(15)
_cell_length_b                   12.595(2)
_cell_length_c                   17.554(3)
_cell_measurement_reflns_used    693
_cell_measurement_temperature    298.00(2)
_cell_measurement_theta_max      30.9830
_cell_measurement_theta_min      3.2100
_cell_volume                     1844.7(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.00(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -69.00 113.00   0.50   15.00    --   29.89  54.00 -60.00  364
  2  ω     -4.00  21.00   0.50   15.00    --   29.89  54.00 -90.00   50
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0760505000
_diffrn_orient_matrix_UB_12      0.0246035000
_diffrn_orient_matrix_UB_13      -0.0004936000
_diffrn_orient_matrix_UB_21      -0.0381594000
_diffrn_orient_matrix_UB_22      0.0497961000
_diffrn_orient_matrix_UB_23      -0.0075314000
_diffrn_orient_matrix_UB_31      0.0021268000
_diffrn_orient_matrix_UB_32      0.0096241000
_diffrn_orient_matrix_UB_33      0.0397997000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0876
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5990
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.993
_diffrn_reflns_theta_max         24.993
_diffrn_reflns_theta_min         2.838
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Rigaku (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99196
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_description       block
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.434
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.1497
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1405P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2132
_refine_ls_wR_factor_ref         0.2842
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1597
_reflns_number_total             3233
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc02765d2.cif
_cod_data_source_block           pt01581
_cod_depositor_comments
'Adding full bibliography for 7128811--7128812.cif.'
_cod_original_cell_volume        1844.8(6)
_cod_database_code               7128811
_shelx_shelxl_version_number     2018/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C9(H9)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C12(H12), C4(H4), C15(H15), C25(H25), C16(H16), C14(H14), C3(H3),
 C2(H2A), C13(H13), C18(H18), C19(H19), C22(H22), C24(H24), C20(H20), C23(H23)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.126
_oxdiff_exptl_absorpt_empirical_full_min 0.951
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.6781(3) 0.8673(2) 0.55907(17) 0.0671(9) Uani 1 1 d . . . . .
O2 O 0.4048(4) 0.6015(3) 0.61612(18) 0.0762(10) Uani 1 1 d . . . . .
H2 H 0.337546 0.585258 0.645034 0.114 Uiso 1 1 calc GR . . . .
C6 C 0.4253(5) 0.8407(3) 0.6028(2) 0.0494(10) Uani 1 1 d . . . . .
C5 C 0.3505(5) 0.8230(3) 0.6703(2) 0.0534(10) Uani 1 1 d . . . . .
C10 C 0.5275(5) 0.6802(3) 0.7349(2) 0.0537(10) Uani 1 1 d . . . . .
C7 C 0.5921(5) 0.8071(3) 0.5908(2) 0.0525(10) Uani 1 1 d . . . . .
C11 C 0.4339(5) 0.7716(3) 0.7395(2) 0.0515(10) Uani 1 1 d . . . . .
C8 C 0.6469(5) 0.6970(3) 0.6117(2) 0.0532(10) Uani 1 1 d . . . . .
C9 C 0.5507(5) 0.6275(3) 0.6596(2) 0.0570(11) Uani 1 1 d . . . . .
H9 H 0.610730 0.561616 0.670515 0.068 Uiso 1 1 calc R . . . .
C1 C 0.3453(5) 0.8958(3) 0.5424(3) 0.0658(12) Uani 1 1 d . . . . .
H1 H 0.396971 0.910098 0.499005 0.079 Uiso 1 1 calc R . . . .
C12 C 0.4188(5) 0.8157(3) 0.8106(3) 0.0648(12) Uani 1 1 d . . . . .
H12 H 0.356411 0.876303 0.813819 0.078 Uiso 1 1 calc R . . . .
C4 C 0.1940(5) 0.8590(3) 0.6721(3) 0.0658(12) Uani 1 1 d . . . . .
H4 H 0.142061 0.847757 0.715933 0.079 Uiso 1 1 calc R . . . .
C26 C 0.9677(5) 0.5332(4) 0.6527(3) 0.0689(13) Uani 1 1 d . . . . .
C15 C 0.6031(5) 0.6377(4) 0.8020(3) 0.0676(12) Uani 1 1 d . . . . .
H15 H 0.666191 0.577258 0.799411 0.081 Uiso 1 1 calc R . . . .
C25 C 1.0188(5) 0.6104(4) 0.7126(3) 0.0729(13) Uani 1 1 d . . . . .
H25 H 0.970055 0.676658 0.713150 0.088 Uiso 1 1 calc R . . . .
C21 C 1.0485(5) 0.4319(4) 0.6580(3) 0.0740(14) Uani 1 1 d . . . . .
C16 C 0.7810(5) 0.6643(3) 0.5864(3) 0.0684(13) Uani 1 1 d . . . . .
H16 H 0.838937 0.714107 0.561290 0.082 Uiso 1 1 calc R . . . .
C17 C 0.8494(5) 0.5549(4) 0.5940(3) 0.0722(13) Uani 1 1 d . . . . .
C14 C 0.5867(6) 0.6831(4) 0.8720(3) 0.0771(14) Uani 1 1 d . . . . .
H14 H 0.638736 0.653411 0.916111 0.093 Uiso 1 1 calc R . . . .
C3 C 0.1147(6) 0.9104(4) 0.6111(3) 0.0793(14) Uani 1 1 d . . . . .
H3 H 0.009470 0.932632 0.613603 0.095 Uiso 1 1 calc R . . . .
C2 C 0.1897(5) 0.9295(4) 0.5461(3) 0.0795(14) Uani 1 1 d . . . . .
H2A H 0.135725 0.964964 0.504851 0.095 Uiso 1 1 calc R . . . .
C13 C 0.4934(6) 0.7724(4) 0.8769(3) 0.0802(14) Uani 1 1 d . . . . .
H13 H 0.480931 0.803043 0.924175 0.096 Uiso 1 1 calc R . . . .
C18 C 0.8086(6) 0.4762(4) 0.5433(3) 0.0792(14) Uani 1 1 d . . . . .
H18 H 0.728918 0.491328 0.504158 0.095 Uiso 1 1 calc R . . . .
C19 C 0.8745(7) 0.3753(4) 0.5443(4) 0.0858(16) Uani 1 1 d . . . . .
H19 H 0.838540 0.324475 0.508201 0.103 Uiso 1 1 calc R . . . .
C22 C 1.1702(7) 0.4162(5) 0.7168(4) 0.0964(19) Uani 1 1 d . . . . .
H22 H 1.224172 0.351543 0.719219 0.116 Uiso 1 1 calc R . . . .
C24 C 1.1379(7) 0.5843(5) 0.7670(4) 0.0951(17) Uani 1 1 d . . . . .
H24 H 1.170282 0.633787 0.804696 0.114 Uiso 1 1 calc R . . . .
C20 C 0.9973(8) 0.3529(5) 0.6017(5) 0.108(2) Uani 1 1 d . . . . .
H20 H 1.046119 0.286535 0.603456 0.130 Uiso 1 1 calc R . . . .
C23 C 1.2119(8) 0.4874(6) 0.7684(4) 0.112(2) Uani 1 1 d . . . . .
H23 H 1.293167 0.472417 0.806801 0.134 Uiso 1 1 calc R . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5 C6 C7 124.8(4) . . ?
C1 C6 C5 120.0(4) . . ?
C1 C6 C7 115.1(4) . . ?
C6 C5 C11 122.8(4) . . ?
C4 C5 C6 117.7(4) . . ?
C4 C5 C11 119.4(4) . . ?
C11 C10 C9 122.2(4) . . ?
C15 C10 C11 118.7(4) . . ?
C15 C10 C9 119.1(4) . . ?
O1 C7 C6 119.4(3) . . ?
O1 C7 C8 120.6(3) . . ?
C8 C7 C6 119.8(3) . . ?
C10 C11 C5 122.1(3) . . ?
C12 C11 C5 119.0(4) . . ?
C12 C11 C10 118.9(4) . . ?
C7 C8 C9 120.6(3) . . ?
C16 C8 C7 117.4(4) . . ?
C16 C8 C9 122.0(4) . . ?
O2 C9 C10 113.4(3) . . ?
O2 C9 C8 108.4(3) . . ?
C8 C9 C10 110.9(3) . . ?
C2 C1 C6 120.6(4) . . ?
C13 C12 C11 122.0(4) . . ?
C3 C4 C5 121.6(4) . . ?
C21 C26 C25 115.9(4) . . ?
C17 C26 C25 122.8(4) . . ?
C17 C26 C21 121.3(5) . . ?
C14 C15 C10 121.4(4) . . ?
C24 C25 C26 119.4(5) . . ?
C22 C21 C26 118.6(5) . . ?
C22 C21 C20 124.0(5) . . ?
C20 C21 C26 117.4(5) . . ?
C8 C16 C17 126.3(4) . . ?
C26 C17 C16 119.2(5) . . ?
C18 C17 C26 117.5(5) . . ?
C18 C17 C16 123.1(5) . . ?
C15 C14 C13 120.2(4) . . ?
C4 C3 C2 120.4(4) . . ?
C3 C2 C1 119.6(4) . . ?
C14 C13 C12 118.9(5) . . ?
C17 C18 C19 126.0(5) . . ?
C18 C19 C20 117.4(5) . . ?
C23 C22 C21 123.2(6) . . ?
C25 C24 C23 122.1(6) . . ?
C19 C20 C21 120.4(5) . . ?
C22 C23 C24 120.8(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C7 1.218(4) . ?
O2 C9 1.416(5) . ?
C6 C5 1.410(5) . ?
C6 C7 1.496(5) . ?
C6 C1 1.384(6) . ?
C5 C11 1.491(5) . ?
C5 C4 1.391(5) . ?
C10 C11 1.400(5) . ?
C10 C9 1.508(5) . ?
C10 C15 1.390(6) . ?
C7 C8 1.495(5) . ?
C11 C12 1.383(6) . ?
C8 C9 1.501(5) . ?
C8 C16 1.314(6) . ?
C1 C2 1.380(6) . ?
C12 C13 1.379(6) . ?
C4 C3 1.369(6) . ?
C26 C25 1.465(7) . ?
C26 C21 1.443(6) . ?
C26 C17 1.387(6) . ?
C15 C14 1.374(6) . ?
C25 C24 1.354(7) . ?
C21 C22 1.395(7) . ?
C21 C20 1.438(8) . ?
C16 C17 1.493(6) . ?
C17 C18 1.353(6) . ?
C14 C13 1.378(7) . ?
C3 C2 1.376(7) . ?
C18 C19 1.386(7) . ?
C19 C20 1.398(8) . ?
C22 C23 1.299(9) . ?
C24 C23 1.368(8) . ?
