#------------------------------------------------------------------------------
#$Date: 2025-03-04 20:24:28 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298019 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/40/7134021.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_7134021
loop_
_publ_author_name
'Haldar, Rajashi'
'Naskar, Sudip'
'Jana, Bapan'
'Mandal, Dipankar'
'Shanmugam, Maheswaran'
_publ_section_title
;
 Harnessing thermal waste with a poling-free molecular pyroelectric
 zinc(II) complex.
;
_journal_issue                   2
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              318
_journal_page_last               321
_journal_paper_doi               10.1039/d4cc06054g
_journal_volume                  61
_journal_year                    2024
_chemical_formula_moiety         'C30 H24 N6 Zn1, 2(Cl1 O4)'
_chemical_formula_sum            'C30 H24 Cl2 N6 O10 Zn'
_chemical_formula_weight         764.82
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-07-09
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-08-07 deposited with the CCDC.	2024-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   10.5944(9)
_cell_length_b                   10.5944(9)
_cell_length_c                   16.2218(14)
_cell_measurement_reflns_used    1698
_cell_measurement_temperature    400.00(10)
_cell_measurement_theta_max      30.0570
_cell_measurement_theta_min      2.1960
_cell_volume                     1576.8(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'PROGRAM:BIS V6.2.16/2021-10-22 && APEX4 2021.4-0                                '
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      400.00(10)
_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   -115.72  16.28   1.00    2.00    --  -15.82 -59.25  20.08  132
  2  ω   -115.72  16.28   1.00    2.00    --  -15.82 -59.25 -84.92  132
  3  φ     19.79 163.79   1.00    2.00  16.41 -15.82 -59.25    --   144
  4  φ    -10.56 141.44   1.00    2.00  75.04 -15.82  31.50    --   152
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0420879000
_diffrn_orient_matrix_UB_12      0.0701258000
_diffrn_orient_matrix_UB_13      0.0177394000
_diffrn_orient_matrix_UB_21      0.0173178000
_diffrn_orient_matrix_UB_22      0.0314080000
_diffrn_orient_matrix_UB_23      -0.0399515000
_diffrn_orient_matrix_UB_31      -0.0624577000
_diffrn_orient_matrix_UB_32      0.0082639000
_diffrn_orient_matrix_UB_33      0.0008962000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1177
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            18182
_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         2.220
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear pinkish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   pinkish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     72
_refine_ls_number_reflns         935
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0881
_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)+(0.1866P)²+0.7139P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2690
_refine_ls_wR_factor_ref         0.3105
_reflns_Friedel_coverage         0.000
_reflns_number_gt                577
_reflns_number_total             935
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc06054g2.cif
_cod_data_source_block           ms_rh_znbpyclo4_400k_autored
_cod_depositor_comments
'Adding full bibliography for 7134019--7134021.cif.'
_cod_original_cell_volume        1576.8(3)
_cod_database_code               7134021
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Zn Cl'
_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_max   0.907
_shelx_estimated_absorpt_t_min   0.836
_reflns_odcompleteness_completeness 94.38
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     32.96
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C12(H12), C14(H14), C13(H13)
;
_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 1.983
_oxdiff_exptl_absorpt_empirical_full_min 0.556
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, 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
Zn1 Zn 0.000000 1.000000 0.750000 0.0754(9) Uani 1 6 d S T P . .
Cl11 Cl 0.333333 0.666667 0.6331(2) 0.1027(13) Uani 1 3 d S T P . .
N11 N -0.0812(6) 0.7990(6) 0.6818(4) 0.0807(16) Uani 1 1 d . . . . .
C11 C -0.0395(6) 0.7074(7) 0.7105(4) 0.0735(16) Uani 1 1 d . . . . .
C15 C -0.1546(8) 0.7684(8) 0.6109(5) 0.094(2) Uani 1 1 d . . . . .
H15 H -0.184386 0.832436 0.592211 0.112 Uiso 1 1 calc R . . . .
C12 C -0.0723(9) 0.5827(8) 0.6681(5) 0.106(2) Uani 1 1 d . . . . .
H12 H -0.045533 0.517596 0.688842 0.127 Uiso 1 1 calc R . . . .
C14 C -0.1883(9) 0.6487(10) 0.5645(6) 0.102(3) Uani 1 1 d . . . . .
H14 H -0.238121 0.631557 0.514794 0.122 Uiso 1 1 calc R . . . .
C13 C -0.1462(10) 0.5551(9) 0.5935(5) 0.119(3) Uani 1 1 d . . . . .
H13 H -0.166971 0.472275 0.563351 0.142 Uiso 1 1 calc R . . . .
O12 O 0.3066(13) 0.7675(18) 0.6613(14) 0.391(12) Uani 1 1 d . . . . .
O11 O 0.333333 0.666667 0.5695(14) 0.50(5) Uani 1 3 d S T P . .
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'
Cl Cl 0.1484 0.1585 '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'
Zn Zn 0.2839 1.4301 '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
N11 Zn1 N11 169.1(3) 3_465 6_556 ?
N11 Zn1 N11 76.3(3) 5_676 2_675 ?
N11 Zn1 N11 96.1(2) 5_676 4_466 ?
N11 Zn1 N11 96.1(2) 3_465 . ?
N11 Zn1 N11 96.1(2) 6_556 4_466 ?
N11 Zn1 N11 76.3(3) 6_556 . ?
N11 Zn1 N11 92.4(3) 6_556 2_675 ?
N11 Zn1 N11 92.4(3) 3_465 5_676 ?
N11 Zn1 N11 76.3(3) 3_465 4_466 ?
N11 Zn1 N11 96.1(2) 6_556 5_676 ?
N11 Zn1 N11 92.4(3) . 4_466 ?
N11 Zn1 N11 169.1(3) . 5_676 ?
N11 Zn1 N11 169.1(3) 2_675 4_466 ?
N11 Zn1 N11 96.1(2) 3_465 2_675 ?
N11 Zn1 N11 96.1(2) . 2_675 ?
O12 Cl11 O12 108.6(11) . 2_665 ?
O12 Cl11 O12 108.6(11) 2_665 3_565 ?
O12 Cl11 O12 108.6(11) . 3_565 ?
O11 Cl11 O12 110.4(11) . 3_565 ?
O11 Cl11 O12 110.4(11) . . ?
O11 Cl11 O12 110.4(11) . 2_665 ?
C11 N11 Zn1 115.1(4) . . ?
C15 N11 Zn1 125.3(5) . . ?
C15 N11 C11 119.3(6) . . ?
N11 C11 C11 116.4(3) . 6_556 ?
N11 C11 C12 120.6(6) . . ?
C12 C11 C11 123.0(5) . 6_556 ?
N11 C15 H15 118.2 . . ?
N11 C15 C14 123.5(7) . . ?
C14 C15 H15 118.2 . . ?
C11 C12 H12 120.5 . . ?
C11 C12 C13 118.9(8) . . ?
C13 C12 H12 120.5 . . ?
C15 C14 H14 121.3 . . ?
C13 C14 C15 117.4(7) . . ?
C13 C14 H14 121.3 . . ?
C12 C13 H13 119.9 . . ?
C14 C13 C12 120.3(7) . . ?
C14 C13 H13 119.9 . . ?
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
Zn1 N11 2.161(6) 3_465 ?
Zn1 N11 2.161(6) 2_675 ?
Zn1 N11 2.161(6) 5_676 ?
Zn1 N11 2.161(6) 6_556 ?
Zn1 N11 2.161(6) . ?
Zn1 N11 2.161(6) 4_466 ?
Cl11 O12 1.317(13) . ?
Cl11 O12 1.317(13) 3_565 ?
Cl11 O12 1.317(13) 2_665 ?
Cl11 O11 1.03(2) . ?
N11 C11 1.336(8) . ?
N11 C15 1.334(9) . ?
C11 C11 1.472(12) 6_556 ?
C11 C12 1.371(9) . ?
C15 H15 0.9300 . ?
C15 C14 1.361(11) . ?
C12 H12 0.9300 . ?
C12 C13 1.391(11) . ?
C14 H14 0.9300 . ?
C14 C13 1.358(12) . ?
C13 H13 0.9300 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 N11 C11 C11 7.4(9) . . . 6_556 ?
Zn1 N11 C11 C12 -173.8(6) . . . . ?
Zn1 N11 C15 C14 171.5(6) . . . . ?
N11 C11 C12 C13 1.8(12) . . . . ?
N11 C15 C14 C13 1.2(12) . . . . ?
C11 N11 C15 C14 -1.1(11) . . . . ?
C11 C11 C12 C13 -179.5(7) 6_556 . . . ?
C11 C12 C13 C14 -1.7(13) . . . . ?
C15 N11 C11 C11 -179.2(7) . . . 6_556 ?
C15 N11 C11 C12 -0.4(10) . . . . ?
C15 C14 C13 C12 0.2(13) . . . . ?
