#------------------------------------------------------------------------------
#$Date: 2023-07-05 13:33:45 +0300 (Wed, 05 Jul 2023) $
#$Revision: 284939 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/24/7062444.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_7062444
loop_
_publ_author_name
'Trivedi, Manoj'
'Singh, Gurmeet'
'Sharma, Raj Kishore'
'Rath, Nigam P.'
'Husain, Ahmad'
_publ_section_title
;
 Synthetic, spectral, structural and catalytic activities of 3-D metal
 format/acetate framework materials for CO2 conversion
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10585
_journal_page_last               10592
_journal_paper_doi               10.1039/D3NJ01463K
_journal_volume                  47
_journal_year                    2023
_chemical_formula_moiety         'C12 H19 Na Ni2 O12'
_chemical_formula_sum            'C12 H19 Na Ni2 O12'
_chemical_formula_weight         495.64
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-07-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-12 deposited with the CCDC.	2023-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.446(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.641(2)
_cell_length_b                   17.787(3)
_cell_length_c                   8.0993(12)
_cell_measurement_reflns_used    4195
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.41
_cell_measurement_theta_min      2.29
_cell_volume                     1920.1(5)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.991
_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  0.0958
_diffrn_reflns_av_unetI/netI     0.0570
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            14709
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.594
_diffrn_reflns_theta_min         2.290
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.041
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.6399
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1130 before and 0.0910 after correction.
The Ratio of minimum to maximum transmission is 0.7423.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_description       block
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.113
_exptl_crystal_size_mid          0.076
_exptl_crystal_size_min          0.051
_refine_diff_density_max         1.692
_refine_diff_density_min         -1.529
_refine_diff_density_rms         0.252
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.349
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2212
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.728
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0686
_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)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1740
_refine_ls_wR_factor_ref         0.1952
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1777
_reflns_number_total             2212
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3nj01463k2.cif
_cod_data_source_block           15_a
_cod_depositor_comments
'Adding full bibliography for 7062444--7062445.cif.'
_cod_database_code               7062444
_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   0.903
_shelx_estimated_absorpt_t_min   0.802
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O4-H4
 0.8 with sigma of 0.01
3.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C)
;
_olex2_submission_special_instructions 'No special instructions were received'
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'
'-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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.20738(4) 0.30583(3) 0.04284(7) 0.0185(3) Uani 1 1 d . . . . .
Na1 Na 0.500000 0.10561(15) 0.250000 0.0251(6) Uani 1 2 d S T P . .
O1 O 0.2865(2) 0.2774(2) 0.2952(5) 0.0300(8) Uani 1 1 d . . . . .
O2 O 0.3628(3) 0.1825(2) 0.2231(5) 0.0307(8) Uani 1 1 d . . . . .
O3 O 0.1194(2) 0.40016(18) 0.0617(4) 0.0251(7) Uani 1 1 d . . . . .
O4 O 0.0714(3) 0.5073(2) 0.1374(5) 0.0391(9) Uani 1 1 d D . . . .
O5 O 0.3197(2) 0.3654(2) 0.0427(5) 0.0322(8) Uani 1 1 d . . . . .
O6 O 0.3927(2) 0.2692(2) -0.0329(5) 0.0314(8) Uani 1 1 d . . . . .
C1 C 0.3449(3) 0.2215(3) 0.3368(6) 0.0229(9) Uani 1 1 d . . . . .
C2 C 0.3976(4) 0.2012(3) 0.5332(7) 0.0300(11) Uani 1 1 d . . . . .
H2A H 0.398297 0.146443 0.546409 0.045 Uiso 1 1 calc GR . . . .
H2B H 0.362258 0.223926 0.600508 0.045 Uiso 1 1 calc GR . . . .
H2C H 0.466655 0.220044 0.581373 0.045 Uiso 1 1 calc GR . . . .
C3 C 0.1375(3) 0.4537(3) 0.1701(7) 0.0262(10) Uani 1 1 d . . . . .
C4 C 0.2344(4) 0.4598(3) 0.3344(8) 0.0405(13) Uani 1 1 d . . . . .
H4A H 0.234867 0.423623 0.425999 0.061 Uiso 1 1 calc GR . . . .
H4B H 0.241483 0.510869 0.383895 0.061 Uiso 1 1 calc GR . . . .
H4C H 0.290245 0.449077 0.301257 0.061 Uiso 1 1 calc GR . . . .
C5 C 0.3882(3) 0.3375(3) 0.0037(6) 0.0255(10) Uani 1 1 d . . . . .
C6 C 0.4676(4) 0.3891(3) -0.0026(8) 0.0417(13) Uani 1 1 d . . . . .
H6A H 0.459910 0.394112 -0.128160 0.063 Uiso 1 1 calc GR . . . .
H6B H 0.533980 0.368362 0.072117 0.063 Uiso 1 1 calc GR . . . .
H6C H 0.460827 0.438658 0.044193 0.063 Uiso 1 1 calc GR . . . .
H4 H 0.000000 0.500000 0.000000 0.05(3) Uiso 1 2 d DS T P . .
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'
O O 0.0106 0.0060 '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'
Ni Ni 0.3393 1.1124 '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
Ni1 Ni1 Na1 124.31(4) 7 7 ?
O1 Ni1 Ni1 86.49(10) . 7 ?
O1 Ni1 Na1 145.97(10) . 7 ?
O1 Ni1 O2 169.48(14) . 7 ?
O1 Ni1 O3 103.89(13) . . ?
O1 Ni1 O5 90.35(15) . . ?
O1 Ni1 O6 88.65(16) . 7 ?
O2 Ni1 Ni1 83.07(10) 7 7 ?
O2 Ni1 Na1 43.41(10) 7 7 ?
O2 Ni1 O3 86.52(13) 7 . ?
O3 Ni1 Ni1 169.52(9) . 7 ?
O3 Ni1 Na1 45.31(9) . 7 ?
O5 Ni1 Ni1 85.23(11) . 7 ?
O5 Ni1 Na1 105.01(11) . 7 ?
O5 Ni1 O2 90.03(16) . 7 ?
O5 Ni1 O3 96.04(13) . . ?
O5 Ni1 O6 169.59(14) . 7 ?
O6 Ni1 Ni1 84.37(11) 7 7 ?
O6 Ni1 Na1 81.29(11) 7 7 ?
O6 Ni1 O2 89.07(16) 7 7 ?
O6 Ni1 O3 94.25(14) 7 . ?
Ni1 Na1 Ni1 124.29(8) 8_556 7 ?
O2 Na1 Ni1 35.06(9) . 7 ?
O2 Na1 Ni1 35.06(9) 2_655 8_556 ?
O2 Na1 Ni1 106.14(12) 2_655 7 ?
O2 Na1 Ni1 106.14(12) . 8_556 ?
O2 Na1 O2 109.3(2) . 2_655 ?
O2 Na1 O3 110.00(13) 2_655 7 ?
O2 Na1 O3 72.98(12) 2_655 8_556 ?
O2 Na1 O3 72.98(12) . 7 ?
O2 Na1 O3 110.00(13) . 8_556 ?
O2 Na1 O4 150.75(12) . 3_545 ?
O2 Na1 O4 88.26(14) . 4_545 ?
O2 Na1 O4 88.26(14) 2_655 3_545 ?
O2 Na1 O4 150.75(12) 2_655 4_545 ?
O3 Na1 Ni1 39.63(8) 7 7 ?
O3 Na1 Ni1 144.10(11) 7 8_556 ?
O3 Na1 Ni1 39.63(8) 8_556 8_556 ?
O3 Na1 Ni1 144.10(11) 8_556 7 ?
O3 Na1 O3 175.1(2) 7 8_556 ?
O4 Na1 Ni1 118.65(9) 3_545 7 ?
O4 Na1 Ni1 101.58(8) 3_545 8_556 ?
O4 Na1 Ni1 118.65(9) 4_545 8_556 ?
O4 Na1 Ni1 101.58(8) 4_545 7 ?
O4 Na1 O3 79.15(12) 4_545 8_556 ?
O4 Na1 O3 97.24(13) 4_545 7 ?
O4 Na1 O3 97.24(13) 3_545 8_556 ?
O4 Na1 O3 79.15(12) 3_545 7 ?
O4 Na1 O4 86.6(2) 4_545 3_545 ?
C1 O1 Ni1 121.8(3) . . ?
Ni1 O2 Na1 101.53(15) 7 . ?
C1 O2 Ni1 124.4(3) . 7 ?
C1 O2 Na1 132.4(3) . . ?
Ni1 O3 Na1 95.06(13) . 7 ?
C3 O3 Ni1 133.2(3) . . ?
C3 O3 Na1 128.5(3) . 7 ?
Na1 O4 H4 94.82(19) 3_455 . ?
C3 O4 Na1 149.0(3) . 3_455 ?
C3 O4 H4 113.9(3) . . ?
C5 O5 Ni1 122.6(3) . . ?
C5 O6 Ni1 123.8(3) . 7 ?
O1 C1 O2 124.0(4) . . ?
O1 C1 C2 117.9(4) . . ?
O2 C1 C2 118.1(4) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O3 C3 O4 119.4(4) . . ?
O3 C3 C4 122.0(4) . . ?
O4 C3 C4 118.6(4) . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O5 C5 C6 118.2(5) . . ?
O6 C5 O5 124.0(4) . . ?
O6 C5 C6 117.8(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 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
Ni1 Ni1 2.5885(11) 7 ?
Ni1 Na1 3.3712(14) 7 ?
Ni1 O1 1.953(3) . ?
Ni1 O2 1.977(4) 7 ?
Ni1 O3 2.159(3) . ?
Ni1 O5 1.956(3) . ?
Ni1 O6 1.958(3) 7 ?
Na1 O2 2.364(4) 2_655 ?
Na1 O2 2.364(4) . ?
Na1 O3 2.406(3) 8_556 ?
Na1 O3 2.406(3) 7 ?
Na1 O4 2.402(4) 3_545 ?
Na1 O4 2.402(4) 4_545 ?
O1 C1 1.262(6) . ?
O2 C1 1.264(6) . ?
O3 C3 1.247(6) . ?
O4 C3 1.306(6) . ?
O4 H4 1.176(3) . ?
O5 C5 1.270(6) . ?
O6 C5 1.260(6) . ?
C1 C2 1.497(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.494(6) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 C6 1.499(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
