#------------------------------------------------------------------------------
#$Date: 2020-09-06 11:14:23 +0300 (Sun, 06 Sep 2020) $
#$Revision: 255958 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/69/7126928.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_7126928
loop_
_publ_author_name
'Xu, Wei-Jian'
'Zeng, Ying'
'Yuan, Wei'
'Zhang, Wei-Xiong'
'Chen, Xiao-Ming'
_publ_section_title
;
 A large room-temperature entropy change in a new hybrid ferroelastic with
 an unconventional bond-switching mechanism.
;
_journal_issue                   69
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10054
_journal_page_last               10057
_journal_paper_doi               10.1039/d0cc04092d
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '0.5(C12 H4 Co2 N12 Na2 O2), 2(C3 H11 N2)'
_chemical_formula_sum            'C12 H24 Co N10 Na O'
_chemical_formula_weight         406.33
_space_group_crystal_system      orthorhombic
_space_group_IT_number           59
_space_group_name_Hall           '-P 2ab 2a'
_space_group_name_H-M_alt        'P m m n :2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-11 deposited with the CCDC.	2020-07-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.4803(3)
_cell_length_b                   12.4172(9)
_cell_length_c                   9.5901(6)
_cell_measurement_reflns_used    2845
_cell_measurement_temperature    333(2)
_cell_measurement_theta_max      30.3020
_cell_measurement_theta_min      2.6750
_cell_volume                     1009.85(10)
_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      333(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4491
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.968
_diffrn_reflns_theta_min         2.684
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41404
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'CrysAlisPro 1.171.38.40t (Rigaku Oxford Diffraction, 2015)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1100
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0494
_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)+(0.1025P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1268
_refine_ls_wR_factor_ref         0.1346
_reflns_Friedel_coverage         0.000
_reflns_number_gt                929
_reflns_number_total             1100
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0cc04092d2.cif
_cod_data_source_block           TMC-2_333K
_cod_depositor_comments
'Adding full bibliography for 7126928--7126929.cif.'
_cod_original_sg_symbol_H-M      'P m m n'
_cod_database_code               7126928
_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_max   1.671
_shelx_estimated_absorpt_t_min   0.638
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All N(H,H) groups, All O(H,H) groups
2. Restrained distances
 N4-C4
 1.481 with sigma of 0.002
 C6-C4
 2.451 with sigma of 0.002
 C4-C5
 2.352 with sigma of 0.002
 C6-C5
 2.455 with sigma of 0.002
 C5-N4
 1.459 with sigma of 0.005
 N4-C6
 1.481 with sigma of 0.002
 N4-N5
 1.481 with sigma of 0.002
 N5-C4
 2.451 with sigma of 0.002
 C6-N5
 2.451 with sigma of 0.002
 C5-N5
 2.352 with sigma of 0.002
3. Others
 Fixed Sof: Na1(0.25) N4(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) N5(0.5)
 H5D(0.5) H5E(0.5) C4(0.5) H4A(0.5) H4B(0.5) H4C(0.5) C6(0.5) H6A(0.5) H6B(0.5)
 H6C(0.5) O1(0.25) H1A(0.25) H1B(0.25)
4.a Riding coordinates:
 C5(H5A,H5B,H5C), N5(H5D,H5E), C4(H4A,H4B,H4C)
4.b Rotating group:
 O1(H1A,H1B)
4.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z'
'x+1/2, -y, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z'
'-x-1/2, y, z'
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
Co1 Co 0.7500 0.7500 0.70244(5) 0.0616(3) Uani 1 4 d S T P B .
Na1 Na 0.2500 0.6962(2) 0.3615(3) 0.0706(7) Uani 0.5 2 d S T P . .
N3 N 0.4859(4) 0.7500 0.4885(4) 0.1024(10) Uani 1 2 d S T P B .
C3 C 0.5875(4) 0.7500 0.5664(3) 0.0719(8) Uani 1 2 d S T P . .
C2 C 0.7500 0.5970(4) 0.6999(4) 0.0844(10) Uani 1 2 d S T P . .
C1 C 0.5943(5) 0.7500 0.8434(4) 0.0835(9) Uani 1 2 d S T P . .
N1 N 0.5026(5) 0.7500 0.9299(4) 0.1287(15) Uani 1 2 d S T P B .
N2 N 0.7500 0.5051(4) 0.6928(4) 0.1324(19) Uani 1 2 d S T P B .
N4 N 0.2551(10) 0.4776(3) 0.7831(3) 0.0859(13) Uani 0.5 1 d D . . A -1
C5 C 0.270(2) 0.5609(6) 0.6747(6) 0.237(9) Uani 0.5 1 d D . . A -1
H5A H 0.2050 0.6209 0.7000 0.356 Uiso 0.5 1 d R . . A -1
H5B H 0.3781 0.5842 0.6681 0.356 Uiso 0.5 1 d R . . A -1
H5C H 0.2368 0.5328 0.5863 0.356 Uiso 0.5 1 d R . . A -1
N5 N 0.3072(12) 0.5295(6) 0.9144(5) 0.215(6) Uani 0.5 1 d D . . A -1
H5D H 0.2979 0.4764 0.9867 0.323 Uiso 0.5 1 d R . . A -1
H5E H 0.4145 0.5537 0.9087 0.323 Uiso 0.5 1 d R . . A -1
C4 C 0.3651(12) 0.3905(7) 0.7408(13) 0.192(6) Uani 0.5 1 d D . . A -1
H4A H 0.4565 0.3893 0.7999 0.288 Uiso 0.5 1 d R . . A -1
H4B H 0.3103 0.3231 0.7482 0.288 Uiso 0.5 1 d R . . A -1
H4C H 0.3971 0.4017 0.6459 0.288 Uiso 0.5 1 d R . . A -1
C6 C 0.0912(11) 0.4367(9) 0.7951(13) 0.196(7) Uani 0.5 1 d D . . A -1
H6A H 0.0190 0.4908 0.7630 0.295 Uiso 0.5 1 calc GR . . A -1
H6B H 0.0689 0.4197 0.8907 0.295 Uiso 0.5 1 calc GR . . A -1
H6C H 0.0798 0.3730 0.7391 0.295 Uiso 0.5 1 calc GR . . A -1
O1 O 0.2376(18) 0.7674(12) 0.1451(8) 0.136(5) Uani 0.25 1 d . . . B -1
H1A H 0.1507 0.8398 0.1123 0.204 Uiso 0.25 1 d GR . . B -1
H1B H 0.3429 0.8120 0.0989 0.204 Uiso 0.25 1 d GR . . B -1
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'
Co Co 0.3494 0.9721 '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'
Na Na 0.0362 0.0249 '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
C3 Co1 C3 93.14(18) . 2_665 ?
C3 Co1 C2 89.49(7) . 2_665 ?
C3 Co1 C2 89.49(7) 2_665 2_665 ?
C3 Co1 C2 89.49(7) 2_665 . ?
C3 Co1 C2 89.49(7) . . ?
C2 Co1 C2 178.5(2) . 2_665 ?
C1 Co1 C3 89.12(17) 2_665 2_665 ?
C1 Co1 C3 177.74(13) . 2_665 ?
C1 Co1 C3 177.74(13) 2_665 . ?
C1 Co1 C3 89.12(17) . . ?
C1 Co1 C2 90.53(7) . . ?
C1 Co1 C2 90.53(7) 2_665 2_665 ?
C1 Co1 C2 90.53(7) . 2_665 ?
C1 Co1 C2 90.53(7) 2_665 . ?
C1 Co1 C1 88.6(2) . 2_665 ?
Na1 Na1 N3 74.07(7) 2_565 . ?
Na1 Na1 N3 74.07(7) 2_565 2_565 ?
Na1 Na1 N2 168.23(10) 2_565 5_666 ?
Na1 Na1 O1 67.0(4) 2_565 . ?
N3 Na1 N3 110.45(19) . 2_565 ?
N3 Na1 N2 111.76(9) 2_565 5_666 ?
N3 Na1 N2 111.76(9) . 5_666 ?
O1 Na1 N3 108.3(5) . 2_565 ?
O1 Na1 N3 113.0(4) . . ?
O1 Na1 N2 101.3(4) . 5_666 ?
Na1 N3 Na1 31.86(13) 2_565 . ?
C3 N3 Na1 161.47(17) . . ?
C3 N3 Na1 161.47(17) . 2_565 ?
N3 C3 Co1 177.5(3) . . ?
N2 C2 Co1 177.3(3) . . ?
N1 C1 Co1 178.9(4) . . ?
C2 N2 Na1 171.7(3) . 5_666 ?
C5 N4 N5 105.52(18) . . ?
C5 N4 C4 105.28(18) . . ?
C5 N4 C6 112.2(2) . . ?
N5 N4 C4 111.24(19) . . ?
N5 N4 C6 111.25(19) . . ?
C6 N4 C4 111.11(19) . . ?
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
Co1 C3 1.898(3) . ?
Co1 C3 1.898(3) 2_665 ?
Co1 C2 1.900(5) 2_665 ?
Co1 C2 1.900(5) . ?
Co1 C1 1.890(4) 2_665 ?
Co1 C1 1.890(4) . ?
Na1 Na1 1.337(5) 2_565 ?
Na1 N3 2.435(3) . ?
Na1 N3 2.435(3) 2_565 ?
Na1 N2 2.553(6) 5_666 ?
Na1 O1 2.259(6) . ?
N3 Na1 2.435(3) 2_565 ?
N3 C3 1.141(5) . ?
C2 N2 1.143(7) . ?
C1 N1 1.137(5) . ?
N2 Na1 2.553(6) 5_666 ?
N4 C5 1.473(3) . ?
N4 N5 1.4820(19) . ?
N4 C4 1.4844(19) . ?
N4 C6 1.4843(19) . ?
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
N5 H5E N1 0.96 2.56 3.204(8) 124.8 .
