#------------------------------------------------------------------------------
#$Date: 2024-12-06 19:27:04 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296450 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/93/7249387.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_7249387
loop_
_publ_author_name
'Wu, Si-Tong'
'Ruan, Zhijun'
'Tian, Zhengfang'
'Shi, Le'
'Yang, Jiong'
'Shao, Dong'
_publ_section_title
;
 Construction, structures, and magnetic studies of two cobalt(ii) and
 nickel(ii) coordination polymers displaying bex topology
;
_journal_issue                   41
_journal_name_full               CrystEngComm
_journal_page_first              5850
_journal_page_last               5858
_journal_paper_doi               10.1039/D4CE00935E
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C11 H11 N Ni O6'
_chemical_formula_sum            'C11 H11 N Ni O6'
_chemical_formula_weight         311.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-12
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-12 deposited with the CCDC.	2024-09-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.954(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.078(2)
_cell_length_b                   9.7734(14)
_cell_length_c                   7.2286(11)
_cell_measurement_reflns_used    7165
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.42
_cell_volume                     1175.8(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.981
_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  0.0568
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            9881
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.417
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.673
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5051
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1450 before and 0.0724 after correction.
The Ratio of minimum to maximum transmission is 0.6774.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.652
_refine_diff_density_min         -2.151
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     94
_refine_ls_number_reflns         1410
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0555
_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)+(0.0647P)²+9.1590P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1397
_refine_ls_wR_factor_ref         0.1404
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1363
_reflns_number_total             1410
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00935e2.cif
_cod_data_source_block           Ni
_cod_depositor_comments
'Adding full bibliography for 7249387--7249388.cif.'
_cod_database_code               7249387
_shelx_shelxl_version_number     2017/1
_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   0.864
_shelx_estimated_absorpt_t_min   0.812
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C5-O2 \\sim C5-O4
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C5) \\sim
Ueq: with sigma of 0 and sigma for terminal atoms of 0.01
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C5) = Uanis(C4) = Uanis(C3) = Uanis(C2)
Uanis(O2) = Uanis(O4)
4. Others
 Sof(O4)=0.5*(1-FVAR(2))
 Sof(O2)=0.5*FVAR(2)
 Fixed Sof: H4B(0.5) H4A(0.5)
5.a Rotating group:
 O1(H1A,H1B)
5.b Secondary CH2 refined with riding coordinates:
 C4(H4B,H4A)
5.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C1(H1), C2(H2)
;
_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, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
Ni1 Ni 0.24894(3) 0.500000 0.59425(8) 0.0182(2) Uani 1 2 d S T P . .
O5 O 0.17339(14) 0.6112(3) 1.3696(4) 0.0254(5) Uani 1 1 d . . . . .
O3 O 0.1511(6) 0.500000 0.7151(8) 0.0353(16) Uani 1 2 d S T P A .
O1 O 0.30338(16) 0.6460(3) 0.7825(4) 0.0312(6) Uani 1 1 d . . . . .
H1A H 0.310458 0.645214 0.903716 0.047 Uiso 1 1 d R U . . .
H1B H 0.324452 0.721557 0.758077 0.047 Uiso 1 1 d R U . . .
N1 N 0.3388(2) 0.500000 0.4455(6) 0.0233(8) Uani 1 2 d S T P A .
C8 C 0.0716(3) 0.500000 1.1380(6) 0.0199(9) Uani 1 2 d S T P . .
C9 C 0.1452(3) 0.500000 1.2974(6) 0.0192(9) Uani 1 2 d S T P . .
C6 C 0.0739(3) 0.500000 0.9461(7) 0.0235(10) Uani 1 2 d S T P A .
C7 C 0.0019(3) 0.500000 0.8099(7) 0.0237(10) Uani 1 2 d S T P . .
H7 H 0.003076 0.500000 0.681926 0.028 Uiso 1 2 calc R U P . .
C1 C 0.3667(2) 0.6171(5) 0.3875(6) 0.0354(9) Uani 1 1 d . . . . .
H1 H 0.348126 0.699582 0.425407 0.043 Uiso 1 1 calc R U . A .
C5 C 0.1529(4) 0.500000 0.8868(9) 0.0518(9) Uani 1 2 d DS T P . .
C3 C 0.4510(4) 0.500000 0.2163(9) 0.0518(9) Uani 1 2 d S T P . .
C2 C 0.4218(3) 0.6202(7) 0.2741(6) 0.0518(9) Uani 1 1 d . . . . .
H2 H 0.439176 0.703725 0.236442 0.062 Uiso 1 1 calc R U . . .
C4 C 0.5135(4) 0.500000 0.0980(9) 0.0518(9) Uani 1 2 d S T P . .
H4B H 0.547291 0.579886 0.132841 0.062 Uiso 0.5 1 calc R U P . .
H4A H 0.547291 0.420114 0.132841 0.062 Uiso 0.5 1 calc R U P . .
O2 O 0.16(4) 0.500000 0.71(3) 0.0386(17) Uani 0.024(14) 2 d DS TU P A 1
O4 O 0.2145(3) 0.4603(6) 1.0114(8) 0.0386(17) Uani 0.488(7) 1 d D U P A 2
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'
N N 0.0061 0.0033 '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'
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
O5 Ni1 O5 61.33(14) 6_564 1_554 ?
O5 Ni1 C9 30.69(7) 1_554 1_554 ?
O5 Ni1 C9 30.69(7) 6_564 1_554 ?
O3 Ni1 O5 85.0(2) . 6_564 ?
O3 Ni1 O5 85.0(2) . 1_554 ?
O3 Ni1 N1 174.0(3) . . ?
O3 Ni1 C9 82.8(3) . 1_554 ?
O1 Ni1 O5 165.85(11) 6_565 1_554 ?
O1 Ni1 O5 165.85(11) . 6_564 ?
O1 Ni1 O5 104.96(11) 6_565 6_564 ?
O1 Ni1 O5 104.96(11) . 1_554 ?
O1 Ni1 O3 90.51(18) 6_565 . ?
O1 Ni1 O3 90.51(18) . . ?
O1 Ni1 O1 88.45(16) . 6_565 ?
O1 Ni1 N1 93.80(11) . . ?
O1 Ni1 N1 93.80(11) 6_565 . ?
O1 Ni1 C9 135.40(8) 6_565 1_554 ?
O1 Ni1 C9 135.40(8) . 1_554 ?
N1 Ni1 O5 89.83(12) . 1_554 ?
N1 Ni1 O5 89.83(12) . 6_564 ?
N1 Ni1 C9 91.15(15) . 1_554 ?
O2 Ni1 O5 86(10) . 6_564 ?
O2 Ni1 O5 86(10) . 1_554 ?
O2 Ni1 O3 1(10) . . ?
O2 Ni1 O1 90(9) . . ?
O2 Ni1 O1 90(9) . 6_565 ?
O2 Ni1 N1 175(10) . . ?
O2 Ni1 C9 84(10) . 1_554 ?
C9 O5 Ni1 89.2(2) . 1_556 ?
C5 O3 Ni1 126.1(8) . . ?
Ni1 O1 H1A 127.8 . . ?
Ni1 O1 H1B 127.8 . . ?
H1A O1 H1B 104.4 . . ?
C1 N1 Ni1 121.4(2) . . ?
C1 N1 Ni1 121.4(2) 6_565 . ?
C1 N1 C1 117.0(5) 6_565 . ?
C6 C8 C9 123.9(4) . . ?
C7 C8 C9 116.3(4) 5_567 . ?
C7 C8 C6 119.8(4) 5_567 . ?
O5 C9 Ni1 60.1(2) 6_565 1_556 ?
O5 C9 Ni1 60.1(2) . 1_556 ?
O5 C9 O5 120.1(4) 6_565 . ?
O5 C9 C8 119.8(2) 6_565 . ?
O5 C9 C8 119.7(2) . . ?
C8 C9 Ni1 170.0(3) . 1_556 ?
C8 C6 C5 120.6(5) . . ?
C7 C6 C8 119.1(4) . . ?
C7 C6 C5 120.3(5) . . ?
C8 C7 C6 121.1(4) 5_567 . ?
C8 C7 H7 119.4 5_567 . ?
C6 C7 H7 119.4 . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.8(5) . . ?
C2 C1 H1 118.6 . . ?
O3 C5 C6 117.7(7) . . ?
O3 C5 O2 6(10) . . ?
O3 C5 O4 122.6(7) . . ?
O3 C5 O4 122.6(7) . 6_565 ?
O2 C5 C6 124(10) . . ?
O4 C5 C6 116.5(5) . . ?
O4 C5 C6 116.5(5) 6_565 . ?
O4 C5 O4 35.2(5) . 6_565 ?
C2 C3 C2 117.1(6) 6_565 . ?
C2 C3 C4 121.5(3) . . ?
C2 C3 C4 121.5(3) 6_565 . ?
C1 C2 H2 119.9 . . ?
C3 C2 C1 120.2(6) . . ?
C3 C2 H2 119.9 . . ?
C3 C4 H4B 107.9 . . ?
C3 C4 H4A 107.9 . . ?
C4 C4 C3 117.6(7) 5_665 . ?
C4 C4 H4B 107.9 5_665 . ?
C4 C4 H4A 107.9 5_665 . ?
H4B C4 H4A 107.2 . . ?
C5 O2 Ni1 133(10) . . ?
O4 O4 C5 72.4(3) 6_565 . ?
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 O5 2.132(3) 6_564 ?
Ni1 O5 2.132(3) 1_554 ?
Ni1 O3 2.052(8) . ?
Ni1 O1 2.046(3) . ?
Ni1 O1 2.046(3) 6_565 ?
Ni1 N1 2.062(4) . ?
Ni1 C9 2.457(5) 1_554 ?
Ni1 O2 1.9(5) . ?
O5 C9 1.254(3) . ?
O3 C5 1.234(8) . ?
O1 H1A 0.8574 . ?
O1 H1B 0.8570 . ?
N1 C1 1.342(5) . ?
N1 C1 1.342(5) 6_565 ?
C8 C9 1.503(6) . ?
C8 C6 1.396(6) . ?
C8 C7 1.390(6) 5_567 ?
C6 C7 1.391(7) . ?
C6 C5 1.505(7) . ?
C7 H7 0.9300 . ?
C1 H1 0.9300 . ?
C1 C2 1.380(5) . ?
C5 O2 1.28(2) . ?
C5 O4 1.282(9) . ?
C5 O4 1.282(9) 6_565 ?
C3 C2 1.377(7) 6_565 ?
C3 C2 1.377(7) . ?
C3 C4 1.511(8) . ?
C2 H2 0.9300 . ?
C4 C4 1.388(13) 5_665 ?
C4 H4B 0.9700 . ?
C4 H4A 0.9700 . ?
O4 O4 0.775(12) 6_565 ?
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
Ni1 O5 C9 O5 -4.5(4) 1_556 . . 6_565 ?
Ni1 O5 C9 C8 168.5(4) 1_556 . . . ?
Ni1 O3 C5 C6 180.000(1) . . . . ?
Ni1 O3 C5 O2 0.00(12) . . . . ?
Ni1 O3 C5 O4 21.0(4) . . . 6_565 ?
Ni1 O3 C5 O4 -21.0(4) . . . . ?
Ni1 N1 C1 C2 -174.3(3) . . . . ?
O3 C5 O2 Ni1 180.00(13) . . . . ?
O3 C5 O4 O4 101.7(4) . . . 6_565 ?
N1 C1 C2 C3 -0.4(7) . . . . ?
C8 C6 C7 C8 0.000(2) . . . 5_567 ?
C8 C6 C5 O3 180.000(2) . . . . ?
C8 C6 C5 O2 180.00(8) . . . . ?
C8 C6 C5 O4 19.8(3) . . . . ?
C8 C6 C5 O4 -19.8(3) . . . 6_565 ?
C9 C8 C6 C7 180.000(2) . . . . ?
C9 C8 C6 C5 0.000(2) . . . . ?
C6 C8 C9 O5 -93.5(4) . . . 6_565 ?
C6 C8 C9 O5 93.5(4) . . . . ?
C6 C5 O2 Ni1 180.00(3) . . . . ?
C6 C5 O4 O4 -99.1(3) . . . 6_565 ?
C7 C8 C9 O5 86.5(4) 5_567 . . 6_565 ?
C7 C8 C9 O5 -86.5(4) 5_567 . . . ?
C7 C8 C6 C7 0.000(2) 5_567 . . . ?
C7 C8 C6 C5 180.000(2) 5_567 . . . ?
C7 C6 C5 O3 0.000(2) . . . . ?
C7 C6 C5 O2 0.00(10) . . . . ?
C7 C6 C5 O4 -160.2(3) . . . . ?
C7 C6 C5 O4 160.2(3) . . . 6_565 ?
C1 N1 C1 C2 -0.3(8) 6_565 . . . ?
C5 C6 C7 C8 180.000(1) . . . 5_567 ?
C2 C3 C2 C1 1.1(9) 6_565 . . . ?
C2 C3 C4 C4 90.6(6) 6_565 . . 5_665 ?
C2 C3 C4 C4 -90.6(6) . . . 5_665 ?
C4 C3 C2 C1 -177.8(5) . . . . ?
