#------------------------------------------------------------------------------
#$Date: 2024-07-05 16:11:50 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292763 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/30/7133095.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_7133095
loop_
_publ_author_name
'Iwai, Yuudai'
'Nakaya, Manabu'
'Tsuji, Yuta'
'Le Ouay, Benjamin'
'Ohba, Masaaki'
'Ohtani, Ryo'
_publ_section_title
;
 Giant anisotropic thermal expansion of copper-cyanido flat layers with
 flexible copper nodes.
;
_journal_issue                   51
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6512
_journal_page_last               6515
_journal_paper_doi               10.1039/d4cc01232a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         '0.5(C4 Cu4 N8), C8 H20 N'
_chemical_formula_sum            'C10 H20 Cu2 N5'
_chemical_formula_weight         337.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           72
_space_group_name_Hall           '-I 2 2c'
_space_group_name_H-M_alt        'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-04-14
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-03-04 deposited with the CCDC.	2024-05-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7778(10)
_cell_length_b                   8.2376(6)
_cell_length_c                   12.5337(8)
_cell_measurement_reflns_used    4315
_cell_measurement_temperature    350.0
_cell_measurement_theta_max      25.79
_cell_measurement_theta_min      2.76
_cell_volume                     1525.77(18)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      350.0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5790
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         2.757
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.775
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5834
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0980 before and 0.0629 after correction.
The Ratio of minimum to maximum transmission is 0.7824.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       block
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.332
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.326
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     47
_refine_ls_number_reflns         779
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0323
_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)+(0.0430P)²+1.0916P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0930
_reflns_Friedel_coverage         0.000
_reflns_number_gt                667
_reflns_number_total             779
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc01232a2.cif
_cod_data_source_block           230413_teacu_350k
_cod_depositor_comments
'Adding full bibliography for 7133093--7133099.cif.'
_cod_database_code               7133095
_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_max   0.784
_shelx_estimated_absorpt_t_min   0.459
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1, y+1, -z+1/2'
'x+1, -y+1, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x-1/2, -y-1/2, z'
'-x-1/2, y-1/2, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x, -y, z+1/2'
'-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
Cu1 Cu 0.65780(3) 0.10087(6) 0.500000 0.0850(3) Uani 1 2 d S T P . .
C1 C 0.7096(2) 0.3111(4) 0.500000 0.0779(9) Uani 1 2 d S T P . .
N3 N 0.500000 0.500000 0.250000 0.0777(11) Uani 1 4 d S T P . .
N1 N 0.7531(3) 0.4261(4) 0.500000 0.0956(10) Uani 1 2 d S T P . .
N2 N 0.5364(2) 0.0268(5) 0.500000 0.1009(11) Uani 1 2 d S T P . .
C2 C 0.5576(2) 0.3953(4) 0.1769(3) 0.1107(12) Uani 1 1 d . . . . .
H2A H 0.517599 0.332929 0.131238 0.133 Uiso 1 1 calc R U . . .
H2B H 0.593032 0.466117 0.131407 0.133 Uiso 1 1 calc R U . . .
C3 C 0.6206(3) 0.2802(7) 0.2320(5) 0.186(3) Uani 1 1 d . . . . .
H3A H 0.656251 0.223833 0.179729 0.279 Uiso 1 1 calc R U . . .
H3B H 0.586190 0.203169 0.272658 0.279 Uiso 1 1 calc R U . . .
H3C H 0.659837 0.339821 0.278800 0.279 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'
Cu Cu 0.3201 1.2651 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1.00 -1.00 0.00 0.0480
-1.00 -1.00 -1.00 0.1110
0.00 -1.00 1.00 0.1040
0.00 -1.00 0.00 0.0600
-1.00 0.00 0.00 0.0460
1.00 0.00 0.00 0.0160
-1.00 0.00 1.00 0.0910
1.00 0.00 -1.00 0.1310
0.00 0.00 -1.00 0.1660
-1.00 1.00 1.00 0.0680
0.00 1.00 -1.00 0.0930
0.00 1.00 1.00 0.0760
0.00 1.00 0.00 0.0200
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 Cu1 N1 113.69(15) . 3_646 ?
C1 Cu1 N2 132.63(16) . . ?
N2 Cu1 N1 113.69(15) . 3_646 ?
N1 C1 Cu1 169.7(3) . . ?
C2 N3 C2 111.9(3) 2_665 7_545 ?
C2 N3 C2 110.8(3) . 7_545 ?
C2 N3 C2 105.8(3) 8_455 7_545 ?
C2 N3 C2 110.8(3) 8_455 2_665 ?
C2 N3 C2 111.9(3) . 8_455 ?
C2 N3 C2 105.8(3) . 2_665 ?
C1 N1 Cu1 171.7(3) . 3_656 ?
N2 N2 Cu1 176.4(5) 9_656 . ?
N3 C2 H2A 108.4 . . ?
N3 C2 H2B 108.4 . . ?
H2A C2 H2B 107.5 . . ?
C3 C2 N3 115.5(3) . . ?
C3 C2 H2A 108.4 . . ?
C3 C2 H2B 108.4 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
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
Cu1 C1 1.893(4) . ?
Cu1 N1 1.952(4) 3_646 ?
Cu1 N2 1.896(3) . ?
C1 N1 1.144(5) . ?
N3 C2 1.519(3) . ?
N3 C2 1.519(3) 2_665 ?
N3 C2 1.519(3) 8_455 ?
N3 C2 1.519(3) 7_545 ?
N2 N2 1.162(7) 9_656 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.497(6) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
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
N1 Cu1 C1 N1 0.0 3_646 . . . ?
N2 Cu1 C1 N1 180.0 . . . . ?
C2 N3 C2 C3 -179.9(4) 2_665 . . . ?
C2 N3 C2 C3 -58.5(3) 7_545 . . . ?
C2 N3 C2 C3 59.4(3) 8_455 . . . ?
