#------------------------------------------------------------------------------
#$Date: 2017-04-05 12:36:24 +0300 (Wed, 05 Apr 2017) $
#$Revision: 195036 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/78/7227812.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_7227812
loop_
_publ_author_name
'Lu, Yang'
'Wang, Zhongxia'
'Chen, Hai-Peng'
'Ge, Jia-Zhen'
_publ_section_title
;
 High temperature structural phase transition and dielectric relaxation in
 an organic--inorganic hybrid compound: (4-methylpiperidinium)CdCl3
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              1896
_journal_paper_doi               10.1039/C7CE00053G
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C6 H14 Cd Cl3 N'
_chemical_formula_sum            'C6 H14 Cd Cl3 N'
_chemical_formula_weight         318.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-01 deposited with the CCDC.
2017-03-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.7868(14)
_cell_length_b                   20.823(4)
_cell_length_c                   7.4953(15)
_cell_measurement_reflns_used    1020
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.482
_cell_measurement_theta_min      3.157
_cell_volume                     1059.2(4)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku SCXmini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0807
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6848
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         3.157
_exptl_absorpt_coefficient_mu    2.761
_exptl_absorpt_correction_T_max  0.581
_exptl_absorpt_correction_T_min  0.576
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.000
_exptl_crystal_description       Prism
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         2.209
_refine_diff_density_min         -1.966
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   1.06(10)
_refine_ls_extinction_coef       0.093(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         2407
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0476
_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)+(0.0271P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0909
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2167
_reflns_number_total             2428
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce00053g2.cif
_cod_data_source_block           Y
_cod_depositor_comments
'Adding full bibliography for 7227812--7227813.cif.'
_cod_original_cell_volume        1059.3(4)
_cod_database_code               7227812
_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.
;
_shelx_estimated_absorpt_t_min   0.608
_shelx_estimated_absorpt_t_max   0.608
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, 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
C1 C 0.1831(11) 0.6423(4) 0.6610(17) 0.048(3) Uani 1 1 d . .
H1A H 0.1779 0.6434 0.5317 0.058 Uiso 1 1 calc R U
H1B H 0.0997 0.6765 0.7061 0.058 Uiso 1 1 calc R U
C2 C 0.1083(12) 0.5793(4) 0.7257(13) 0.041(3) Uani 1 1 d . .
H2A H -0.0228 0.5723 0.6778 0.049 Uiso 1 1 calc R U
H2B H 0.0975 0.5807 0.8547 0.049 Uiso 1 1 calc R U
C3 C 0.2394(10) 0.5225(4) 0.6732(16) 0.0347(19) Uani 1 1 d . .
H3 H 0.2426 0.5203 0.5426 0.042 Uiso 1 1 calc R U
C4 C 0.4442(12) 0.5362(4) 0.7367(13) 0.044(3) Uani 1 1 d . .
H4A H 0.4449 0.5372 0.8661 0.053 Uiso 1 1 calc R U
H4B H 0.5304 0.5016 0.6989 0.053 Uiso 1 1 calc R U
C5 C 0.5219(11) 0.5981(4) 0.6675(18) 0.045(2) Uani 1 1 d . .
H5A H 0.5330 0.5960 0.5387 0.054 Uiso 1 1 calc R U
H5B H 0.6520 0.6059 0.7164 0.054 Uiso 1 1 calc R U
C6 C 0.1590(15) 0.4584(5) 0.7428(19) 0.080(4) Uani 1 1 d . .
H6A H 0.2352 0.4237 0.6938 0.120 Uiso 1 1 calc R U
H6B H 0.0238 0.4537 0.7074 0.120 Uiso 1 1 calc R U
H6C H 0.1679 0.4575 0.8706 0.120 Uiso 1 1 calc R U
Cd1 Cd 1.05357(7) 0.74576(2) 0.1864(3) 0.0273(2) Uani 1 1 d . .
Cl1 Cl 1.3117(2) 0.64888(9) 0.1674(3) 0.0310(5) Uani 1 1 d . .
Cl2 Cl 0.7982(4) 0.70447(16) -0.0474(3) 0.0331(7) Uani 1 1 d . .
Cl3 Cl 0.7969(4) 0.71107(16) 0.4283(2) 0.0301(7) Uani 1 1 d . .
N1 N 0.3842(10) 0.6526(3) 0.7197(11) 0.045(2) Uani 1 1 d . .
H1C H 0.3854 0.6570 0.8379 0.054 Uiso 1 1 calc R U
H1D H 0.4288 0.6891 0.6726 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'
N N 0.0061 0.0033 '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'
Cd Cd -0.8075 1.2024 '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
N1 C1 C2 110.7(8) . .
C1 C2 C3 113.5(7) . .
C4 C3 C2 108.2(7) . .
C4 C3 C6 112.8(8) . .
C2 C3 C6 112.2(8) . .
C5 C4 C3 112.5(8) . .
C4 C5 N1 109.9(7) . .
Cl2 Cd1 Cl3 177.60(9) . 3_565
Cl2 Cd1 Cl3 86.12(6) . .
Cl3 Cd1 Cl3 91.98(12) 3_565 .
Cl2 Cd1 Cl2 95.85(13) . 3_565
Cl3 Cd1 Cl2 85.85(6) 3_565 3_565
Cl3 Cd1 Cl2 172.78(13) . 3_565
Cl2 Cd1 Cl1 98.67(9) . .
Cl3 Cd1 Cl1 83.24(9) 3_565 .
Cl3 Cd1 Cl1 105.34(9) . .
Cl2 Cd1 Cl1 81.27(9) 3_565 .
Cl2 Cd1 Cl1 80.29(10) . 3_465
Cl3 Cd1 Cl1 97.99(9) 3_565 3_465
Cl3 Cd1 Cl1 81.86(9) . 3_465
Cl2 Cd1 Cl1 91.61(8) 3_565 3_465
Cl1 Cd1 Cl1 172.69(12) . 3_465
Cl2 Cd1 Cd1 49.76(7) . 3_465
Cl3 Cd1 Cd1 127.84(7) 3_565 3_465
Cl3 Cd1 Cd1 49.42(6) . 3_465
Cl2 Cd1 Cd1 127.64(7) 3_565 3_465
Cl1 Cd1 Cd1 133.87(4) . 3_465
Cl1 Cd1 Cd1 50.28(4) 3_465 3_465
Cl2 Cd1 Cd1 132.86(7) . 3_565
Cl3 Cd1 Cd1 49.51(7) 3_565 3_565
Cl3 Cd1 Cd1 132.78(6) . 3_565
Cl2 Cd1 Cd1 49.33(7) 3_565 3_565
Cl1 Cd1 Cd1 52.07(4) . 3_565
Cl1 Cd1 Cd1 123.77(4) 3_465 3_565
Cd1 Cd1 Cd1 174.04(3) 3_465 3_565
Cd1 Cl1 Cd1 77.65(5) . 3_565
Cd1 Cl2 Cd1 80.91(9) . 3_465
Cd1 Cl3 Cd1 81.06(9) 3_465 .
C1 N1 C5 112.9(7) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.450(10) .
C1 C2 1.489(12) .
C2 C3 1.530(11) .
C3 C4 1.496(11) .
C3 C6 1.535(12) .
C4 C5 1.486(12) .
C5 N1 1.522(10) .
Cd1 Cl2 2.610(3) .
Cd1 Cl3 2.613(3) 3_565
Cd1 Cl3 2.616(3) .
Cd1 Cl2 2.627(3) 3_565
Cd1 Cl1 2.6756(18) .
Cd1 Cl1 2.7437(19) 3_465
Cd1 Cd1 3.3980(7) 3_465
Cd1 Cd1 3.3980(7) 3_565
Cl1 Cd1 2.7438(18) 3_565
Cl2 Cd1 2.627(3) 3_465
Cl3 Cd1 2.613(3) 3_465
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
_geom_hbond_site_symmetry_A
N1 H1D Cl3 0.89 2.91 3.630(8) 139.0 3_465
N1 H1C Cl1 0.89 2.53 3.392(8) 164.6 1_456
C5 H5B Cl2 0.97 2.89 3.605(11) 131.6 1_556
C1 H1B Cl2 0.97 2.82 3.644(10) 143.5 1_456
C1 H1A Cl1 0.97 2.88 3.803(13) 159.5 1_455
