#------------------------------------------------------------------------------
#$Date: 2019-11-07 21:32:55 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223539 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/40/7234031.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_7234031
loop_
_publ_author_name
'Muthukumar, Pandi'
'Moon, Dohyun'
'Anthony, Savarimuthu Philip'
_publ_section_title
;
 The Co2+/Ni2+ ion-mediated formation of a topochemically converted copper
 coordination polymer: structure-dependent electrocatalytic activity
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6552
_journal_paper_doi               10.1039/C9CE01178A
_journal_volume                  21
_journal_year                    2019
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C10 H11 Cu N O3'
_chemical_formula_sum            'C10 H11 Cu N O3'
_chemical_formula_weight         256.74
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.8480(12)
_cell_length_b                   8.8480(12)
_cell_length_c                   24.929(5)
_cell_measurement_reflns_used    58035
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_volume                     1951.6(5)
_computing_cell_refinement       'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_data_collection
'PAL BL2D-SMDC Program(Shin et.al, 2016)'
_computing_data_reduction        'HKL3000sm(Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'DIAMOND 4(Putx&Brandenburg, 2014)'
_computing_publication_material  'publCIF(Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2018(Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018(Sheldrick, 2018)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Rayonix MX225HS CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.630
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_unetI/netI     0.0373
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            19158
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         2.165
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.600
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'HKL3000sm Scalepack(Otwinowski et.al,2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.165
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details
;
 Flack x determined using 996 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0278
_refine_ls_R_factor_gt           0.0276
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0402P)²+0.4644P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.636
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                2570
_reflns_number_total             2611
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9ce01178a2.cif
_cod_data_source_block           SPA272
_cod_depositor_comments
'Adding full bibliography for 7234031--7234032.cif.'
_cod_original_cell_volume        1951.6(7)
_cod_database_code               7234031
_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_min   0.719
_shelx_estimated_absorpt_t_max   0.850
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+3/4'
'y+1/2, -x+1/2, z+1/4'
'-x+1/2, y+1/2, -z+3/4'
'x+1/2, -y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -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
Cu1 Cu 0.65018(3) 0.31244(4) 0.69014(2) 0.02267(11) Uani 1 1 d . .
O1 O 0.7662(2) 0.4307(2) 0.74298(6) 0.0266(4) Uani 1 1 d . .
O2 O 0.4757(2) 0.2676(2) 0.64525(7) 0.0290(4) Uani 1 1 d . .
O3 O 0.3494(2) 0.3551(3) 0.57430(9) 0.0339(4) Uani 1 1 d . .
N1 N 0.7214(2) 0.4325(2) 0.62801(8) 0.0208(4) Uani 1 1 d . .
H1 H 0.800492 0.372279 0.610701 0.025 Uiso 1 1 calc R U
C1 C 0.9061(3) 0.4773(3) 0.72969(9) 0.0235(5) Uani 1 1 d . .
C2 C 1.0287(4) 0.4527(4) 0.76331(11) 0.0346(7) Uani 1 1 d . .
H2 H 1.014832 0.404869 0.796169 0.042 Uiso 1 1 calc R U
C3 C 1.1716(4) 0.4995(4) 0.74790(13) 0.0441(8) Uani 1 1 d . .
H3 H 1.253031 0.484177 0.770855 0.053 Uiso 1 1 calc R U
C4 C 1.1949(4) 0.5686(4) 0.69876(14) 0.0444(8) Uani 1 1 d . .
H4 H 1.291601 0.597512 0.688279 0.053 Uiso 1 1 calc R U
C5 C 1.0726(3) 0.5942(4) 0.66549(11) 0.0346(6) Uani 1 1 d . .
H5 H 1.087582 0.642029 0.632700 0.042 Uiso 1 1 calc R U
C6 C 0.9274(3) 0.5499(3) 0.68007(9) 0.0244(5) Uani 1 1 d . .
C7 C 0.7939(3) 0.5773(3) 0.64410(10) 0.0276(6) Uani 1 1 d . .
H7A H 0.720654 0.639916 0.662685 0.033 Uiso 1 1 calc R U
H7AB H 0.826673 0.631300 0.612292 0.033 Uiso 1 1 calc R U
C8 C 0.5983(3) 0.4485(3) 0.58791(10) 0.0241(5) Uani 1 1 d . .
H8 H 0.565343 0.554290 0.587606 0.029 Uiso 1 1 calc R U
C9 C 0.4628(3) 0.3498(3) 0.60304(10) 0.0235(5) Uani 1 1 d . .
C10 C 0.6561(4) 0.4083(5) 0.53180(11) 0.0417(8) Uani 1 1 d . .
H10A H 0.571898 0.397093 0.507834 0.062 Uiso 1 1 calc R U
H10B H 0.711594 0.315207 0.533359 0.062 Uiso 1 1 calc R U
H10C H 0.720997 0.487466 0.519026 0.062 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 0.0021 0.0012 '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 0.0044 0.0025 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0080 0.0047 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3383 1.0252 '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
O1 Cu1 O2 97.37(8) 8_666 .
O1 Cu1 O1 78.95(9) 8_666 .
O2 Cu1 O1 154.82(9) . .
O1 Cu1 N1 168.50(9) 8_666 .
O2 Cu1 N1 84.95(8) . .
O1 Cu1 N1 94.13(8) . .
O1 Cu1 O3 100.57(8) 8_666 6_556
O2 Cu1 O3 112.42(9) . 6_556
O1 Cu1 O3 92.69(9) . 6_556
N1 Cu1 O3 88.84(8) . 6_556
O1 Cu1 Cu1 39.81(6) 8_666 8_666
O2 Cu1 Cu1 132.59(6) . 8_666
O1 Cu1 Cu1 39.15(5) . 8_666
N1 Cu1 Cu1 132.75(6) . 8_666
O3 Cu1 Cu1 98.02(6) 6_556 8_666
C1 O1 Cu1 130.78(16) . 8_666
C1 O1 Cu1 118.49(14) . .
Cu1 O1 Cu1 101.04(9) 8_666 .
C9 O2 Cu1 115.21(16) . .
C9 O3 Cu1 132.91(19) . 6_456
C8 N1 C7 114.6(2) . .
C8 N1 Cu1 110.12(15) . .
C7 N1 Cu1 112.84(15) . .
C8 N1 H1 106.2 . .
C7 N1 H1 106.2 . .
Cu1 N1 H1 106.2 . .
O1 C1 C2 121.5(2) . .
O1 C1 C6 118.7(2) . .
C2 C1 C6 119.9(3) . .
C3 C2 C1 119.9(3) . .
C3 C2 H2 120.0 . .
C1 C2 H2 120.0 . .
C4 C3 C2 120.9(3) . .
C4 C3 H3 119.5 . .
C2 C3 H3 119.5 . .
C5 C4 C3 119.1(3) . .
C5 C4 H4 120.5 . .
C3 C4 H4 120.5 . .
C4 C5 C6 121.4(3) . .
C4 C5 H5 119.3 . .
C6 C5 H5 119.3 . .
C5 C6 C1 118.8(3) . .
C5 C6 C7 121.6(2) . .
C1 C6 C7 119.6(2) . .
N1 C7 C6 111.1(2) . .
N1 C7 H7A 109.4 . .
C6 C7 H7A 109.4 . .
N1 C7 H7AB 109.4 . .
C6 C7 H7AB 109.4 . .
H7A C7 H7AB 108.0 . .
N1 C8 C9 110.7(2) . .
N1 C8 C10 110.3(2) . .
C9 C8 C10 110.7(2) . .
N1 C8 H8 108.3 . .
C9 C8 H8 108.3 . .
C10 C8 H8 108.3 . .
O3 C9 O2 124.7(2) . .
O3 C9 C8 118.2(2) . .
O2 C9 C8 117.1(2) . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9432(17) 8_666
Cu1 O2 1.9477(19) .
Cu1 O1 1.9706(18) .
Cu1 N1 1.981(2) .
Cu1 O3 2.331(2) 6_556
Cu1 Cu1 3.0209(8) 8_666
O1 C1 1.346(3) .
O2 C9 1.284(3) .
O3 C9 1.234(3) .
N1 C8 1.485(3) .
N1 C7 1.488(3) .
N1 H1 0.9800 .
C1 C2 1.388(4) .
C1 C6 1.406(3) .
C2 C3 1.385(5) .
C2 H2 0.9300 .
C3 C4 1.385(5) .
C3 H3 0.9300 .
C4 C5 1.383(5) .
C4 H4 0.9300 .
C5 C6 1.392(4) .
C5 H5 0.9300 .
C6 C7 1.503(4) .
C7 H7A 0.9700 .
C7 H7AB 0.9700 .
C8 C9 1.530(4) .
C8 C10 1.531(4) .
C8 H8 0.9800 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
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
_geom_hbond_publ_flag
N1 H1 O2 0.98 1.99 2.922(3) 158.1 6_556 yes
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
Cu1 O1 C1 C2 9.4(4) 8_666
Cu1 O1 C1 C2 -129.7(2) .
Cu1 O1 C1 C6 -171.73(19) 8_666
Cu1 O1 C1 C6 49.2(3) .
O1 C1 C2 C3 178.7(3) .
C6 C1 C2 C3 -0.1(5) .
C1 C2 C3 C4 -1.1(5) .
C2 C3 C4 C5 1.6(6) .
C3 C4 C5 C6 -1.0(5) .
C4 C5 C6 C1 -0.2(5) .
C4 C5 C6 C7 180.0(3) .
O1 C1 C6 C5 -178.1(3) .
C2 C1 C6 C5 0.7(4) .
O1 C1 C6 C7 1.7(4) .
C2 C1 C6 C7 -179.5(3) .
C8 N1 C7 C6 -174.0(2) .
Cu1 N1 C7 C6 59.0(2) .
C5 C6 C7 N1 118.7(3) .
C1 C6 C7 N1 -61.1(3) .
C7 N1 C8 C9 -136.4(2) .
Cu1 N1 C8 C9 -7.9(2) .
C7 N1 C8 C10 100.7(3) .
Cu1 N1 C8 C10 -130.9(2) .
Cu1 O3 C9 O2 -23.1(4) 6_456
Cu1 O3 C9 C8 157.30(19) 6_456
Cu1 O2 C9 O3 -168.2(2) .
Cu1 O2 C9 C8 11.4(3) .
N1 C8 C9 O3 177.7(2) .
C10 C8 C9 O3 -59.6(3) .
N1 C8 C9 O2 -2.0(3) .
C10 C8 C9 O2 120.8(3) .
