#------------------------------------------------------------------------------
#$Date: 2021-11-06 20:52:35 +0200 (Sat, 06 Nov 2021) $
#$Revision: 270376 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/89/7128956.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_7128956
loop_
_publ_author_name
'Wu, Pingfan'
'Li, Jincheng'
'Xiao, Zicheng'
'Zhao, Yanchao'
'Wang, Yu'
'Xiao, Bowen'
'Huang, Bo'
_publ_section_title
;
 Ir-based electrocatalysts promoted by TME-substituted
 polyoxovanadate-derived vanadium carbide for efficient hydrogen evolution
 and oxygen evolution.
;
_journal_issue                   80
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10395
_journal_page_last               10398
_journal_paper_doi               10.1039/d1cc03559b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C10 H18 Na2 O25 V6, 2(H2 O)'
_chemical_formula_sum            'C10 H22 Na2 O27 V6'
_chemical_formula_weight         925.89
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-05-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-06-29 deposited with the CCDC.	2021-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                105.368(5)
_cell_angle_beta                 101.641(6)
_cell_angle_gamma                94.300(6)
_cell_formula_units_Z            1
_cell_length_a                   8.4801(13)
_cell_length_b                   8.4744(13)
_cell_length_c                   10.9285(17)
_cell_measurement_reflns_used    7283
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      60.683
_cell_measurement_theta_min      6.202
_cell_volume                     734.8(2)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_collection       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 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      193.0
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker smart apex 2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34138
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10169
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         60.813
_diffrn_reflns_theta_min         6.202
_exptl_absorpt_coefficient_mu    11.062
_exptl_absorpt_correction_T_max  0.7519
_exptl_absorpt_correction_T_min  0.5261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1630 before and 0.0850 after correction.
The Ratio of minimum to maximum transmission is 0.6997.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_description       block
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.596
_refine_diff_density_min         -0.867
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0502
_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)+(0.0832P)²+0.8228P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1449
_refine_ls_wR_factor_ref         0.1486
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2973
_reflns_number_total             3314
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc03559b2.cif
_cod_data_source_block           20210512chen_czpz0108_0m
_cod_depositor_comments          'Adding full bibliography for 7128956.cif.'
_cod_database_code               7128956
_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.
;
_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, All O(H,H) groups
2.a Free rotating group:
 O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C19(H19A,H19B), C26(H26A,H26B)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -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
V1 V 0.53890(7) 1.14621(7) -0.13825(5) 0.02126(18) Uani 1 1 d . . . . .
V2 V 0.59323(7) 0.79343(7) -0.13152(5) 0.02213(18) Uani 1 1 d . . . . .
V3 V 0.74789(7) 1.12226(7) 0.11365(5) 0.02195(18) Uani 1 1 d . . . . .
O5 O 0.7318(3) 1.2219(3) -0.0125(2) 0.0240(5) Uani 1 1 d . . . . .
O6 O 0.5491(3) 1.2576(3) -0.2347(3) 0.0289(6) Uani 1 1 d . . . . .
O7 O 0.5685(3) 0.7009(3) 0.0128(2) 0.0209(5) Uani 1 1 d . . . . .
O8 O 0.7983(3) 0.9188(3) -0.0018(2) 0.0217(5) Uani 1 1 d . . . . .
O10 O 0.6905(3) 0.9635(3) 0.2168(2) 0.0228(5) Uani 1 1 d . . . . .
O11 O 0.3786(3) 0.7384(3) -0.2051(2) 0.0256(5) Uani 1 1 d . . . . .
O12 O 0.6121(3) 0.9580(3) -0.2152(2) 0.0259(5) Uani 1 1 d . . . . .
O13 O 0.6714(3) 0.6479(3) -0.2151(2) 0.0291(6) Uani 1 1 d . . . . .
O14 O 0.9286(3) 1.1908(3) 0.2016(3) 0.0301(6) Uani 1 1 d . . . . .
O15 O 0.5000 1.0000 0.0000 0.0197(7) Uani 1 2 d S T P . .
C16 C 0.8114(5) 0.8645(4) 0.2566(3) 0.0266(7) Uani 1 1 d . . . . .
H16A H 0.7722 0.8053 0.3139 0.032 Uiso 1 1 calc R . . . .
H16B H 0.9126 0.9381 0.3078 0.032 Uiso 1 1 calc R . . . .
C19 C 0.9146(4) 0.8259(4) 0.0521(4) 0.0260(7) Uani 1 1 d . . . . .
H19A H 1.0150 0.9014 0.1027 0.031 Uiso 1 1 calc R . . . .
H19B H 0.9431 0.7428 -0.0198 0.031 Uiso 1 1 calc R . . . .
C26 C 0.6961(4) 0.6179(4) 0.0651(3) 0.0249(7) Uani 1 1 d . . . . .
H26A H 0.7225 0.5337 -0.0072 0.030 Uiso 1 1 calc R . . . .
H26B H 0.6577 0.5604 0.1237 0.030 Uiso 1 1 calc R . . . .
C2 C 0.8492(4) 0.7385(4) 0.1407(4) 0.0259(7) Uani 1 1 d . . . . .
C5 C 0.9803(5) 0.6417(5) 0.1931(4) 0.0357(9) Uani 1 1 d . . . . .
H5A H 1.0811 0.7171 0.2373 0.054 Uiso 1 1 calc GR . . . .
H5B H 1.0002 0.5551 0.1205 0.054 Uiso 1 1 calc GR . . . .
H5C H 0.9432 0.5911 0.2551 0.054 Uiso 1 1 calc GR . . . .
Na1 Na 0.5618(3) 1.3571(2) -0.41749(18) 0.0497(5) Uani 1 1 d . . . . .
O2 O 0.6606(4) 1.4965(4) -0.5611(3) 0.0424(7) Uani 1 1 d . . . . .
O3 O 0.7205(4) 1.1621(4) -0.5142(3) 0.0456(8) Uani 1 1 d . . . . .
O1 O 0.9587(5) 1.7101(5) -0.4665(3) 0.0574(9) Uani 1 1 d . . . . .
H1A H 1.0315 1.7300 -0.3937 0.086 Uiso 1 1 d G . . . .
H1B H 0.8826 1.7683 -0.4459 0.086 Uiso 1 1 d G . . . .
O0AA O 0.6806(5) 0.8733(4) -0.4521(3) 0.0539(9) Uani 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0148 0.0070 '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'
Na Na 0.1116 0.0924 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.2866 1.7327 '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
V3 V1 V2 64.989(19) . . ?
O5 V1 V2 87.93(8) . . ?
O5 V1 V3 33.15(8) . . ?
O5 V1 O7 86.87(10) . 2_675 ?
O5 V1 O10 157.75(11) . 2_675 ?
O5 V1 O15 80.38(8) . . ?
O6 V1 V2 137.49(10) . . ?
O6 V1 V3 136.00(10) . . ?
O6 V1 O5 102.89(13) . . ?
O6 V1 O7 97.86(12) . 2_675 ?
O6 V1 O10 97.91(13) . 2_675 ?
O6 V1 O12 103.69(13) . . ?
O6 V1 O15 173.98(10) . . ?
O7 V1 V2 123.97(7) 2_675 . ?
O7 V1 V3 81.98(7) 2_675 . ?
O7 V1 O15 77.16(7) 2_675 . ?
O10 V1 V2 81.94(7) 2_675 . ?
O10 V1 V3 125.36(7) 2_675 . ?
O10 V1 O7 82.54(10) 2_675 2_675 ?
O10 V1 O15 78.22(7) 2_675 . ?
O12 V1 V2 34.06(8) . . ?
O12 V1 V3 85.78(8) . . ?
O12 V1 O5 92.87(12) . . ?
O12 V1 O7 157.93(11) . 2_675 ?
O12 V1 O10 89.76(11) . 2_675 ?
O12 V1 O15 81.04(8) . . ?
O15 V1 V2 47.014(15) . . ?
O15 V1 V3 47.276(17) . . ?
V3 V2 V1 65.137(19) 2_675 . ?
O7 V2 V1 124.72(7) . . ?
O7 V2 V3 81.77(7) . 2_675 ?
O7 V2 O8 82.62(10) . . ?
O7 V2 O15 78.09(7) . . ?
O8 V2 V1 81.02(7) . . ?
O8 V2 V3 123.54(7) . 2_675 ?
O8 V2 O15 77.14(7) . . ?
O11 V2 V1 85.64(8) . . ?
O11 V2 V3 34.64(8) . 2_675 ?
O11 V2 O7 91.02(11) . . ?
O11 V2 O8 158.18(11) . . ?
O11 V2 O12 92.29(12) . . ?
O11 V2 O15 81.13(8) . . ?
O12 V2 V1 32.80(8) . . ?
O12 V2 V3 87.91(8) . 2_675 ?
O12 V2 O7 156.66(11) . . ?
O12 V2 O8 85.81(11) . . ?
O12 V2 O15 79.61(8) . . ?
O13 V2 V1 135.11(10) . . ?
O13 V2 V3 137.28(10) . 2_675 ?
O13 V2 O7 99.42(12) . . ?
O13 V2 O8 98.73(12) . . ?
O13 V2 O11 102.91(13) . . ?
O13 V2 O12 102.34(13) . . ?
O13 V2 O15 175.36(10) . . ?
O15 V2 V1 46.839(16) . . ?
O15 V2 V3 46.588(15) . 2_675 ?
V1 V3 V2 65.46(2) . 2_675 ?
O5 V3 V1 34.63(8) . . ?
O5 V3 V2 86.47(8) . 2_675 ?
O5 V3 O8 91.35(11) . . ?
O5 V3 O10 159.84(11) . . ?
O5 V3 O11 93.73(12) . 2_675 ?
O5 V3 O15 82.40(8) . . ?
O8 V3 V1 83.04(7) . . ?
O8 V3 V2 125.67(7) . 2_675 ?
O8 V3 O10 82.77(10) . . ?
O8 V3 O15 78.59(7) . . ?
O10 V3 V1 125.24(7) . . ?
O10 V3 V2 81.48(7) . 2_675 ?
O10 V3 O15 77.55(7) . . ?
O11 V3 V1 88.68(8) 2_675 . ?
O11 V3 V2 33.05(8) 2_675 2_675 ?
O11 V3 O8 157.37(11) 2_675 . ?
O11 V3 O10 84.94(11) 2_675 . ?
O11 V3 O15 80.25(8) 2_675 . ?
O14 V3 V1 138.16(10) . . ?
O14 V3 V2 135.26(10) . 2_675 ?
O14 V3 O5 103.78(13) . . ?
O14 V3 O8 97.91(13) . . ?
O14 V3 O10 96.13(12) . . ?
O14 V3 O11 102.25(13) . 2_675 ?
O14 V3 O15 173.06(10) . . ?
O15 V3 V1 47.813(16) . . ?
O15 V3 V2 47.290(17) . 2_675 ?
V3 O5 V1 112.23(13) . . ?
V1 O6 Na1 165.40(16) . . ?
V2 O7 V1 110.35(11) . 2_675 ?
C26 O7 V1 118.6(2) . 2_675 ?
C26 O7 V2 118.8(2) . . ?
V3 O8 V2 109.86(11) . . ?
C19 O8 V2 118.3(2) . . ?
C19 O8 V3 119.3(2) . . ?
V1 O10 V3 108.80(11) 2_675 . ?
C16 O10 V1 118.3(2) . 2_675 ?
C16 O10 V3 118.2(2) . . ?
V2 O11 V3 112.30(12) . 2_675 ?
V1 O12 V2 113.14(13) . . ?
V2 O13 Na1 137.38(15) . 1_545 ?
V1 O15 V1 180.0 . 2_675 ?
V1 O15 V2 93.85(2) 2_675 . ?
V1 O15 V2 86.15(2) 2_675 2_675 ?
V1 O15 V2 93.85(2) . 2_675 ?
V1 O15 V2 86.15(2) . . ?
V2 O15 V2 180.0 . 2_675 ?
V3 O15 V1 84.91(2) . . ?
V3 O15 V1 95.09(2) . 2_675 ?
V3 O15 V1 84.91(2) 2_675 2_675 ?
V3 O15 V1 95.09(2) 2_675 . ?
V3 O15 V2 86.12(2) 2_675 . ?
V3 O15 V2 93.88(2) . . ?
V3 O15 V2 93.88(2) 2_675 2_675 ?
V3 O15 V2 86.12(2) . 2_675 ?
V3 O15 V3 180.0 2_675 . ?
O10 C16 C2 112.6(3) . . ?
O8 C19 C2 111.9(3) . . ?
O7 C26 C2 111.7(3) . . ?
C16 C2 C5 108.5(3) . . ?
C19 C2 C16 110.5(3) . . ?
C19 C2 C26 110.7(3) . . ?
C19 C2 C5 108.5(3) . . ?
C26 C2 C16 109.7(3) . . ?
C26 C2 C5 108.9(3) . . ?
O6 Na1 O13 79.76(10) . 1_565 ?
O6 Na1 Na1 145.93(12) . 2_684 ?
O6 Na1 O2 161.68(15) . . ?
O6 Na1 O0AA 86.42(12) . 2_674 ?
O13 Na1 Na1 80.55(9) 1_565 2_684 ?
O2 Na1 O6 104.27(12) 2_684 . ?
O2 Na1 O13 77.97(10) 2_684 1_565 ?
O2 Na1 O13 88.01(11) . 1_565 ?
O2 Na1 Na1 44.17(9) 2_684 2_684 ?
O2 Na1 Na1 42.07(9) . 2_684 ?
O2 Na1 O2 86.23(13) 2_684 . ?
O2 Na1 O3 149.57(14) 2_684 . ?
O2 Na1 O0AA 110.87(12) . 2_674 ?
O2 Na1 O0AA 76.64(13) 2_684 2_674 ?
O3 Na1 O6 97.29(12) . . ?
O3 Na1 O13 127.57(14) . 1_565 ?
O3 Na1 Na1 116.74(11) . 2_684 ?
O3 Na1 O2 79.35(13) . . ?
O3 Na1 O0AA 83.64(13) . 2_674 ?
O0AA Na1 O13 147.00(12) 2_674 1_565 ?
O0AA Na1 Na1 95.37(12) 2_674 2_684 ?
Na1 O2 Na1 93.77(13) 2_684 . ?
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
V1 V2 3.0764(9) . ?
V1 V3 3.0235(9) . ?
V1 O5 1.856(3) . ?
V1 O6 1.600(3) . ?
V1 O7 2.032(2) 2_675 ?
V1 O10 2.004(3) 2_675 ?
V1 O12 1.812(2) . ?
V1 O15 2.2492(6) . ?
V2 V3 3.0627(9) 2_675 ?
V2 O7 1.977(2) . ?
V2 O8 2.023(2) . ?
V2 O11 1.806(3) . ?
V2 O12 1.874(2) . ?
V2 O13 1.601(2) . ?
V2 O15 2.2556(6) . ?
V3 V2 3.0627(9) 2_675 ?
V3 O5 1.786(2) . ?
V3 O8 1.981(2) . ?
V3 O10 2.060(2) . ?
V3 O11 1.882(3) 2_675 ?
V3 O14 1.608(3) . ?
V3 O15 2.2300(6) . ?
O6 Na1 2.383(3) . ?
O7 V1 2.032(2) 2_675 ?
O7 C26 1.439(4) . ?
O8 C19 1.437(4) . ?
O10 V1 2.004(3) 2_675 ?
O10 C16 1.445(4) . ?
O11 V3 1.882(3) 2_675 ?
O13 Na1 2.787(3) 1_545 ?
O15 V1 2.2492(6) 2_675 ?
O15 V2 2.2556(6) 2_675 ?
O15 V3 2.2299(6) 2_675 ?
C16 C2 1.532(5) . ?
C19 C2 1.526(5) . ?
C26 C2 1.527(5) . ?
C2 C5 1.539(5) . ?
Na1 O13 2.787(3) 1_565 ?
Na1 Na1 3.486(3) 2_684 ?
Na1 O2 2.340(4) 2_684 ?
Na1 O2 2.434(4) . ?
Na1 O3 2.375(4) . ?
Na1 O0AA 2.610(5) 2_674 ?
O2 Na1 2.340(4) 2_684 ?
O0AA Na1 2.610(5) 2_674 ?
