#------------------------------------------------------------------------------
#$Date: 2019-11-24 17:31:42 +0200 (Sun, 24 Nov 2019) $
#$Revision: 238841 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/80/7238019.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_7238019
loop_
_publ_author_name
'Li, Wang'
'Zeng, Ying'
'Shu, Xia'
'He, Chun-Ting'
'Du, Zi-Yi'
'Zhang, Wei-Xiong'
'Chen, Xiao-Ming'
_publ_section_title
;
 Isostructural phase transition and tunable water rotation within a unique
 solid rotor system
;
_journal_issue                   42
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              13176
_journal_paper_doi               10.1039/C9TC04765D
_journal_volume                  7
_journal_year                    2019
_chemical_formula_sum            'C16 H38 Br3 N O7 Zn'
_chemical_formula_weight         661.57
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-08-06 deposited with the CCDC.	2019-09-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   14.0180(12)
_cell_length_b                   14.0180(12)
_cell_length_c                   11.1505(19)
_cell_measurement_reflns_used    6959
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.82
_cell_volume                     1897.6(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0632
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5315
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.995
_diffrn_reflns_theta_min         2.906
_exptl_absorpt_coefficient_mu    5.741
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_refine_diff_density_max         0.926
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details
; 
 Twinning involves inversion, so Flack parameter cannot be determined 
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     84
_refine_ls_number_reflns         1621
_refine_ls_number_restraints     129
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0534
_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)+70.7212P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1247
_reflns_Friedel_coverage         1.000
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                1591
_reflns_number_total             1621
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9tc04765d2.cif
_cod_data_source_block           1
_cod_original_cell_volume        1897.6(5)
_cod_database_code               7238019
_shelx_shelxl_version_number     2014/7
_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. 
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
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 0.2390(4) 0.47641(10) 0.00054(15) 0.0181(4) Uani 1 1 d . . . . .
Zn1 Zn 0.3333 0.6667 0.0472(2) 0.0111(6) Uani 1 3 d S T P . .
O1W O 0.3333 0.6667 0.2329(14) 0.021(4) Uani 1 3 d S T P . .
H1WA H 0.3520 0.6135 0.2616 0.025 Uiso 0.125(7) 1 d R U P A 1
H1WB H 0.3865 0.7385 0.2616 0.025 Uiso 0.125(7) 1 d R U P A 1
H1WC H 0.3853 0.6464 0.2619 0.025 Uiso 0.208(7) 1 d R U P A 2
H1WD H 0.3536 0.7389 0.2619 0.025 Uiso 0.208(7) 1 d R U P A 2
O1 O 0.565(2) 0.7280(19) 0.426(3) 0.024(3) Uani 0.38(2) 1 d D U P A 1
O2 O 0.3881(17) 0.513(2) 0.385(3) 0.024(3) Uani 0.38(2) 1 d D U P A 1
C1 C 0.5816(18) 0.638(3) 0.409(3) 0.019(3) Uani 0.38(2) 1 d D U P A 1
H1A H 0.5850 0.6072 0.4876 0.023 Uiso 0.38(2) 1 calc R U P A 1
H1B H 0.6533 0.6636 0.3681 0.023 Uiso 0.38(2) 1 calc R U P A 1
C2 C 0.494(2) 0.550(3) 0.336(3) 0.019(3) Uani 0.38(2) 1 d D U P A 1
H2A H 0.4967 0.5773 0.2540 0.023 Uiso 0.38(2) 1 calc R U P A 1
H2B H 0.5073 0.4868 0.3313 0.023 Uiso 0.38(2) 1 calc R U P A 1
C3 C 0.308(2) 0.406(2) 0.349(4) 0.019(3) Uani 0.38(2) 1 d D U P A 1
H3A H 0.3058 0.3530 0.4088 0.023 Uiso 0.38(2) 1 calc R U P A 1
H3B H 0.3304 0.3897 0.2716 0.023 Uiso 0.38(2) 1 calc R U P A 1
C4 C 0.198(2) 0.389(3) 0.337(3) 0.019(3) Uani 0.38(2) 1 d D U P A 1
H4A H 0.1926 0.4195 0.2583 0.023 Uiso 0.38(2) 1 calc R U P A 1
H4B H 0.1453 0.3086 0.3343 0.023 Uiso 0.38(2) 1 calc R U P A 1
O3 O 0.4856(13) 0.6074(10) 0.356(2) 0.024(3) Uani 0.62(2) 1 d D U P A 2
O4 O 0.2700(10) 0.4413(15) 0.418(2) 0.024(3) Uani 0.62(2) 1 d D U P A 2
C7 C 0.4581(12) 0.4962(14) 0.383(2) 0.019(3) Uani 0.62(2) 1 d D U P A 2
H7A H 0.4665 0.4884 0.4700 0.023 Uiso 0.62(2) 1 calc R U P A 2
H7B H 0.5085 0.4780 0.3394 0.023 Uiso 0.62(2) 1 calc R U P A 2
C8 C 0.3420(14) 0.4194(14) 0.346(3) 0.019(3) Uani 0.62(2) 1 d D U P A 2
H8A H 0.3323 0.4302 0.2600 0.023 Uiso 0.62(2) 1 calc R U P A 2
H8B H 0.3242 0.3422 0.3574 0.023 Uiso 0.62(2) 1 calc R U P A 2
C9 C 0.1623(14) 0.3677(12) 0.381(3) 0.019(3) Uani 0.62(2) 1 d D U P A 2
H9A H 0.1349 0.2987 0.4271 0.023 Uiso 0.62(2) 1 calc R U P A 2
H9B H 0.1644 0.3496 0.2952 0.023 Uiso 0.62(2) 1 calc R U P A 2
C10 C 0.5945(15) 0.6792(14) 0.393(3) 0.019(3) Uani 0.62(2) 1 d D U P A 2
H10A H 0.6440 0.6620 0.3464 0.023 Uiso 0.62(2) 1 calc R U P A 2
H10B H 0.6014 0.6641 0.4785 0.023 Uiso 0.62(2) 1 calc R U P A 2
N1 N 0.3333 0.6667 0.5031(16) 0.016(4) Uani 1 3 d S T P . .
H1C H 0.3668 0.6263 0.4726 0.019 Uiso 0.125(7) 1 d R U P A 1
H1D H 0.3737 0.7405 0.4726 0.019 Uiso 0.125(7) 1 d R U P A 1
H1E H 0.2595 0.6332 0.4726 0.019 Uiso 0.125(7) 1 d R U P A 1
H1F H 0.3311 0.6010 0.4745 0.019 Uiso 0.208(7) 1 d R U P A 2
H1G H 0.3990 0.7301 0.4745 0.019 Uiso 0.208(7) 1 d R U P A 2
H1H H 0.2699 0.6689 0.4745 0.019 Uiso 0.208(7) 1 d R U P A 2
C5 C 0.3333 0.6667 0.638(2) 0.020(5) Uani 1 3 d S T P . .
C6 C 0.402(3) 0.613(3) 0.6838(13) 0.020(4) Uani 1 1 d . U . . .
H6A H 0.4704 0.6423 0.6370 0.030 Uiso 1 1 calc R U . . .
H6B H 0.3589 0.5332 0.6742 0.030 Uiso 1 1 calc R U . . .
H6C H 0.4204 0.6314 0.7687 0.030 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'
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
O1W Zn1 Br1 102.69(6) . 2_665
O1W Zn1 Br1 102.69(6) . .
Br1 Zn1 Br1 115.31(5) 2_665 .
O1W Zn1 Br1 102.69(6) . 3_565
Br1 Zn1 Br1 115.31(5) 2_665 3_565
Br1 Zn1 Br1 115.31(5) . 3_565
C4 O1 C1 114(2) 2_665 .
C3 O2 C2 114.7(17) . .
O1 C1 C2 112.6(13) . .
O2 C2 C1 112.4(13) . .
O2 C3 C4 115.4(13) . .
O1 C4 C3 115.9(14) 3_565 .
C10 O3 C7 108.9(14) . .
C9 O4 C8 107.0(15) . .
O3 C7 C8 109.3(11) . .
O4 C8 C7 108.7(11) . .
O4 C9 C10 115.9(11) . 3_565
O3 C10 C9 115.8(11) . 2_665
N1 C5 C6 108.9(10) . 2_665
N1 C5 C6 108.9(10) . 3_565
C6 C5 C6 110.0(10) 2_665 3_565
N1 C5 C6 108.9(10) . .
C6 C5 C6 110.0(10) 2_665 .
C6 C5 C6 110.0(10) 3_565 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Zn1 2.3676(13) .
Zn1 O1W 2.071(16) .
Zn1 Br1 2.3675(13) 2_665
Zn1 Br1 2.3676(13) 3_565
O1 C4 1.403(14) 2_665
O1 C1 1.414(14) .
O2 C3 1.406(14) .
O2 C2 1.413(14) .
C1 C2 1.471(14) .
C3 C4 1.445(14) .
C4 O1 1.403(14) 3_565
O3 C10 1.405(13) .
O3 C7 1.437(13) .
O4 C9 1.398(13) .
O4 C8 1.436(14) .
C7 C8 1.492(13) .
C9 C10 1.435(12) 3_565
C10 C9 1.435(12) 2_665
N1 C5 1.50(3) .
C5 C6 1.573(17) 2_665
C5 C6 1.573(17) 3_565
C5 C6 1.573(17) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O1W H1WC O3 0.96 2.04 2.99(2) 168.6
O1W H1WA O2 0.96 2.20 3.13(4) 160.9
N1 H1C O2 0.96 2.01 2.94(3) 161.4
N1 H1F O4 0.96 2.06 2.98(2) 160.5
