#------------------------------------------------------------------------------
#$Date: 2022-02-08 01:38:37 +0200 (Tue, 08 Feb 2022) $
#$Revision: 272845 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/43/7244355.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_7244355
loop_
_publ_author_name
'Dwivedi, Bhavna'
'Kumar, Sunil'
'Das, Dinabandhu'
_publ_section_title
;
 Selective inclusion of p-xylene by bis-hydrazone compounds
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1161
_journal_page_last               1165
_journal_paper_doi               10.1039/D1CE01569A
_journal_volume                  24
_journal_year                    2022
_chemical_formula_sum            'C28 H18 Br4 N4'
_chemical_formula_weight         730.10
_space_group_crystal_system      tetragonal
_space_group_IT_number           86
_space_group_name_Hall           '-P 4bc'
_space_group_name_H-M_alt        'P 42/n :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-11-22 deposited with the CCDC.	2021-12-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2289(6)
_cell_length_b                   14.2289(6)
_cell_length_c                   13.1662(8)
_cell_measurement_reflns_used    9903
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.70
_cell_measurement_theta_min      2.55
_cell_volume                     2665.6(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Xseed-2017 (Barbour, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-III Photon-II detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            46444
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         28.403
_diffrn_reflns_theta_min         2.107
_diffrn_source                   microfocus
_exptl_absorpt_coefficient_mu    6.064
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5640
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.819
_exptl_crystal_description       Block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.00076(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick, 2018)'
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         3332
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0409P)²+1.5353P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0871
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2383
_reflns_number_total             3332
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1ce01569a2.cif
_cod_data_source_block           Bromo_unsolvated
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        2665.7(3)
_cod_original_sg_symbol_H-M      'P 42/n'
_cod_database_code               7244355
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_min   0.291
_shelx_estimated_absorpt_t_max   0.530
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z'
'y+1/2, -x, z+1/2'
'-x, -y, -z'
'y, -x-1/2, -z-1/2'
'x-1/2, y-1/2, -z'
'-y-1/2, x, -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
Br1 Br 0.10559(3) 0.32030(3) 0.47023(3) 0.07980(15) Uani 1 1 d . . . . .
N1 N 0.17353(15) 0.57025(15) 0.91619(17) 0.0470(5) Uani 1 1 d . . . . .
C1 C 0.21840(17) 0.56767(17) 0.83119(19) 0.0414(6) Uani 1 1 d . . . . .
Br2 Br 0.57972(2) 0.80344(2) 0.80721(3) 0.06320(13) Uani 1 1 d . . . . .
N2 N 0.09948(16) 0.50639(16) 0.92345(18) 0.0512(5) Uani 1 1 d . . . . .
C2 C 0.19109(16) 0.50895(17) 0.74262(19) 0.0391(5) Uani 1 1 d . . . . .
C3 C 0.10202(18) 0.51467(19) 0.7014(2) 0.0465(6) Uani 1 1 d . . . . .
H3 H 0.057828 0.557580 0.729206 0.056 Uiso 1 1 calc R U . . .
C4 C 0.07644(18) 0.4589(2) 0.6204(2) 0.0490(6) Uani 1 1 d . . . . .
H4 H 0.015356 0.463950 0.591781 0.059 Uiso 1 1 calc R U . . .
C5 C 0.14006(19) 0.39620(19) 0.58156(19) 0.0479(6) Uani 1 1 d . . . . .
C6 C 0.23049(19) 0.38936(19) 0.6201(2) 0.0475(6) Uani 1 1 d . . . . .
H6 H 0.274236 0.346090 0.592096 0.057 Uiso 1 1 calc R U . . .
C7 C 0.25528(18) 0.44634(18) 0.69940(19) 0.0451(6) Uani 1 1 d . . . . .
H7 H 0.317410 0.443262 0.725606 0.054 Uiso 1 1 calc R U . . .
C8 C 0.30343(17) 0.62777(17) 0.82437(18) 0.0416(6) Uani 1 1 d . . . . .
C9 C 0.34821(18) 0.65886(18) 0.9120(2) 0.0458(6) Uani 1 1 d . . . . .
H9 H 0.322500 0.643320 0.976407 0.055 Uiso 1 1 calc R U . . .
C10 C 0.42891(18) 0.71159(17) 0.9072(2) 0.0473(6) Uani 1 1 d . . . . .
H10 H 0.458721 0.732530 0.967617 0.057 Uiso 1 1 calc R U . . .
C11 C 0.46607(18) 0.73374(18) 0.8137(2) 0.0479(6) Uani 1 1 d . . . . .
C12 C 0.4227(2) 0.7069(2) 0.7253(2) 0.0557(7) Uani 1 1 d . . . . .
H12 H 0.447648 0.724774 0.661211 0.067 Uiso 1 1 calc R U . . .
C13 C 0.3414(2) 0.6530(2) 0.7314(2) 0.0526(7) Uani 1 1 d . . . . .
H13 H 0.311404 0.633051 0.670649 0.063 Uiso 1 1 calc R U . . .
C15 C 0.03940(18) 0.52966(19) 0.99058(19) 0.0454(6) Uani 1 1 d . . . . .
H15 H 0.047061 0.586284 1.027912 0.054 Uiso 1 1 calc R U . . .
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'
Br Br -0.2901 2.4595 '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'
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
C1 N1 N2 114.5(2) . . ?
N1 C1 C8 116.1(2) . . ?
N1 C1 C2 124.6(2) . . ?
C8 C1 C2 119.3(2) . . ?
C15 N2 N1 112.7(2) . . ?
C3 C2 C7 118.5(2) . . ?
C3 C2 C1 121.0(2) . . ?
C7 C2 C1 120.5(2) . . ?
C4 C3 C2 120.8(2) . . ?
C4 C3 H3 119.6 . . ?
C2 C3 H3 119.6 . . ?
C5 C4 C3 119.3(2) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C4 C5 C6 121.5(2) . . ?
C4 C5 Br1 119.4(2) . . ?
C6 C5 Br1 119.1(2) . . ?
C7 C6 C5 118.5(2) . . ?
C7 C6 H6 120.8 . . ?
C5 C6 H6 120.8 . . ?
C6 C7 C2 121.3(2) . . ?
C6 C7 H7 119.3 . . ?
C2 C7 H7 119.3 . . ?
C13 C8 C9 118.1(2) . . ?
C13 C8 C1 121.4(2) . . ?
C9 C8 C1 120.5(2) . . ?
C10 C9 C8 121.3(2) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C9 C10 C11 119.2(3) . . ?
C9 C10 H10 120.4 . . ?
C11 C10 H10 120.4 . . ?
C12 C11 C10 121.5(2) . . ?
C12 C11 Br2 119.4(2) . . ?
C10 C11 Br2 119.2(2) . . ?
C11 C12 C13 118.6(3) . . ?
C11 C12 H12 120.7 . . ?
C13 C12 H12 120.7 . . ?
C8 C13 C12 121.2(3) . . ?
C8 C13 H13 119.4 . . ?
C12 C13 H13 119.4 . . ?
N2 C15 C15 119.7(3) . 5_567 ?
N2 C15 H15 120.2 . . ?
C15 C15 H15 120.2 5_567 . ?
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
Br1 C5 1.886(3) . ?
N1 C1 1.289(3) . ?
N1 N2 1.395(3) . ?
C1 C8 1.484(3) . ?
C1 C2 1.486(4) . ?
Br2 C11 1.899(3) . ?
N2 C15 1.273(3) . ?
C2 C3 1.381(3) . ?
C2 C7 1.397(4) . ?
C3 C4 1.378(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.370(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(4) . ?
C6 C7 1.368(4) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C13 1.386(4) . ?
C8 C9 1.390(4) . ?
C9 C10 1.373(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.376(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.372(4) . ?
C12 C13 1.389(4) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C15 C15 1.425(5) 5_567 ?
C15 H15 0.9500 . ?
