#------------------------------------------------------------------------------
#$Date: 2024-09-26 00:34:34 +0200 (Thu 26 de Sep de 2024) $
#$Revision: 294893 $
#$URL: svn://www.crystallography.net/cod/cif/7/24/93/7249388.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_7249388
loop_
_publ_author_name
'Shao, Dong'
'Wu, Si-Tong'
'Ruan, Zhijun'
'Tian, Zhengfang'
'Shi, Le'
'Yang, Jiong'
_publ_section_title
;
 Construction, structures, and magnetic studies of two cobalt(II) and
 nickel(II) coordination polymers displaying bex topology
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D4CE00935E
_journal_year                    2024
_chemical_formula_moiety         'C11 H11 Co N O6'
_chemical_formula_sum            'C11 H11 Co N O6'
_chemical_formula_weight         312.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-11
_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                 100.663(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2564(8)
_cell_length_b                   9.8760(15)
_cell_length_c                   16.8793(19)
_cell_measurement_reflns_used    8268
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      26.38
_cell_measurement_theta_min      3.55
_cell_volume                     1188.8(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13182
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.396
_diffrn_reflns_theta_min         2.400
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.466
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6174
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.366
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2436
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.0345
_refine_ls_R_factor_gt           0.0282
_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)+(0.0268P)²+1.3301P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0684
_refine_ls_wR_factor_ref         0.0718
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2131
_reflns_number_total             2436
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ce00935e2.cif
_cod_data_source_block           Co
_cod_database_code               7249388
_shelx_shelxl_version_number     2019/1
_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   0.855
_shelx_estimated_absorpt_t_min   0.778
_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
 O6_$1-H2B_$2
 2.2 with sigma of 0.02
3.a Rotating group:
 O4(H4A,H4B), O2(H2A,H2B)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C10(H10), C6(H6), C9(H9), C7(H7)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Co1 Co 0.64167(4) 0.49026(3) 0.75548(2) 0.01930(10) Uani 1 1 d . . . . .
O6 O -0.2578(2) 0.59943(16) 0.66106(9) 0.0265(3) Uani 1 1 d . . . . .
O1 O -0.1792(2) 0.38690(15) 0.67765(9) 0.0250(3) Uani 1 1 d . . . . .
O4 O 0.5078(2) 0.63753(16) 0.80948(9) 0.0276(3) Uani 1 1 d . . . . .
H4A H 0.397260 0.648223 0.782839 0.041 Uiso 1 1 d R U . . .
H4B H 0.561200 0.713341 0.805852 0.041 Uiso 1 1 d R U . . .
O3 O 0.3989(2) 0.46475(17) 0.66588(9) 0.0295(4) Uani 1 1 d . . . . .
O2 O 0.5562(2) 0.32325(16) 0.80930(10) 0.0310(4) Uani 1 1 d . . . . .
H2A H 0.643648 0.249794 0.816344 0.047 Uiso 1 1 d R U . . .
H2B H 0.450789 0.276093 0.778962 0.047 Uiso 1 1 d R U . . .
O5 O 0.1905(2) 0.6000(2) 0.70766(10) 0.0393(5) Uani 1 1 d . . . . .
N1 N 0.8949(2) 0.50593(19) 0.84106(11) 0.0241(4) Uani 1 1 d . . . . .
C1 C -0.0793(3) 0.5026(2) 0.56922(12) 0.0194(4) Uani 1 1 d . . . . .
C2 C -0.1742(3) 0.4964(2) 0.64117(12) 0.0196(4) Uani 1 1 d . . . . .
C5 C 0.2448(3) 0.5253(2) 0.65716(12) 0.0217(4) Uani 1 1 d . . . . .
C4 C 0.1154(3) 0.5083(2) 0.57647(12) 0.0198(4) Uani 1 1 d . . . . .
C3 C -0.1924(3) 0.4947(2) 0.49326(13) 0.0221(4) Uani 1 1 d . . . . .
H3 H -0.321940 0.491454 0.488916 0.026 Uiso 1 1 calc R U . . .
C8 C 1.2427(3) 0.5315(3) 0.94522(14) 0.0304(5) Uani 1 1 d . . . . .
C10 C 0.9600(3) 0.6250(3) 0.87081(16) 0.0365(6) Uani 1 1 d . . . . .
H10 H 0.886276 0.701395 0.856582 0.044 Uiso 1 1 calc R U . . .
C6 C 1.0048(3) 0.3991(3) 0.86297(15) 0.0348(6) Uani 1 1 d . . . . .
H6 H 0.963832 0.314552 0.842680 0.042 Uiso 1 1 calc R U . . .
C9 C 1.1297(3) 0.6413(3) 0.92133(16) 0.0389(6) Uani 1 1 d . . . . .
H9 H 1.168728 0.727397 0.939550 0.047 Uiso 1 1 calc R U . . .
C7 C 1.1765(3) 0.4074(3) 0.91426(16) 0.0404(6) Uani 1 1 d . . . . .
H7 H 1.247447 0.329626 0.927963 0.048 Uiso 1 1 calc R U . . .
C11 C 1.4286(4) 0.5523(3) 1.00098(17) 0.0468(7) Uani 1 1 d . . . . .
H11A H 1.479612 0.638529 0.987956 0.056 Uiso 1 1 calc R U . . .
H11B H 1.405858 0.558642 1.055704 0.056 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'
Co Co 0.3494 0.9721 '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'
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
O6 Co1 O1 59.11(6) 1_655 1_655 ?
O4 Co1 O6 103.07(6) . 1_655 ?
O4 Co1 O1 161.76(6) . 1_655 ?
O4 Co1 O3 90.12(6) . . ?
O4 Co1 N1 93.86(7) . . ?
O3 Co1 O6 83.22(6) . 1_655 ?
O3 Co1 O1 91.32(6) . 1_655 ?
O3 Co1 N1 176.01(7) . . ?
O2 Co1 O6 155.06(6) . 1_655 ?
O2 Co1 O1 98.59(6) . 1_655 ?
O2 Co1 O4 99.65(7) . . ?
O2 Co1 O3 86.58(7) . . ?
O2 Co1 N1 93.00(7) . . ?
N1 Co1 O6 95.61(7) . 1_655 ?
N1 Co1 O1 84.82(6) . 1_655 ?
C2 O6 Co1 92.21(12) . 1_455 ?
C2 O1 Co1 88.14(12) . 1_455 ?
Co1 O4 H4A 109.3 . . ?
Co1 O4 H4B 109.4 . . ?
H4A O4 H4B 104.5 . . ?
C5 O3 Co1 129.40(14) . . ?
Co1 O2 H2A 114.8 . . ?
Co1 O2 H2B 115.7 . . ?
H2A O2 H2B 98.2 . . ?
C10 N1 Co1 121.55(15) . . ?
C10 N1 C6 116.27(19) . . ?
C6 N1 Co1 121.96(15) . . ?
C4 C1 C2 122.55(18) . . ?
C3 C1 C2 117.50(18) . . ?
C3 C1 C4 119.86(19) . . ?
O6 C2 C1 119.81(18) . . ?
O1 C2 O6 120.54(19) . . ?
O1 C2 C1 119.50(18) . . ?
O3 C5 C4 116.37(18) . . ?
O5 C5 O3 126.24(19) . . ?
O5 C5 C4 117.37(18) . . ?
C1 C4 C5 122.17(19) . . ?
C3 C4 C1 118.84(19) 3_566 . ?
C3 C4 C5 118.90(18) 3_566 . ?
C1 C3 C4 121.30(19) . 3_566 ?
C1 C3 H3 119.4 . . ?
C4 C3 H3 119.4 3_566 . ?
C9 C8 C7 116.2(2) . . ?
C9 C8 C11 119.4(2) . . ?
C7 C8 C11 124.3(2) . . ?
N1 C10 H10 118.2 . . ?
N1 C10 C9 123.6(2) . . ?
C9 C10 H10 118.2 . . ?
N1 C6 H6 118.3 . . ?
N1 C6 C7 123.4(2) . . ?
C7 C6 H6 118.3 . . ?
C8 C9 H9 119.7 . . ?
C10 C9 C8 120.5(2) . . ?
C10 C9 H9 119.7 . . ?
C8 C7 H7 120.0 . . ?
C6 C7 C8 120.0(2) . . ?
C6 C7 H7 120.0 . . ?
C8 C11 H11A 108.2 . . ?
C8 C11 H11B 108.2 . . ?
C11 C11 C8 116.3(3) 3_867 . ?
C11 C11 H11A 108.2 3_867 . ?
C11 C11 H11B 108.2 3_867 . ?
H11A C11 H11B 107.4 . . ?
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
Co1 O6 2.1597(16) 1_655 ?
Co1 O1 2.2559(15) 1_655 ?
Co1 O4 2.0536(15) . ?
Co1 O3 2.1136(14) . ?
Co1 O2 2.0346(16) . ?
Co1 N1 2.1225(17) . ?
O6 C2 1.261(3) . ?
O1 C2 1.249(3) . ?
O4 H4A 0.8506 . ?
O4 H4B 0.8504 . ?
O3 C5 1.253(3) . ?
O2 H2A 0.9569 . ?
O2 H2B 0.9586 . ?
O5 C5 1.245(3) . ?
N1 C10 1.331(3) . ?
N1 C6 1.333(3) . ?
C1 C2 1.504(3) . ?
C1 C4 1.396(3) . ?
C1 C3 1.391(3) . ?
C5 C4 1.514(3) . ?
C4 C3 1.393(3) 3_566 ?
C3 H3 0.9300 . ?
C8 C9 1.374(3) . ?
C8 C7 1.383(4) . ?
C8 C11 1.510(3) . ?
C10 H10 0.9300 . ?
C10 C9 1.372(3) . ?
C6 H6 0.9300 . ?
C6 C7 1.381(3) . ?
C9 H9 0.9300 . ?
C7 H7 0.9300 . ?
C11 C11 1.467(5) 3_867 ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
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
Co1 O6 C2 O1 -0.15(19) 1_455 . . . ?
Co1 O6 C2 C1 175.48(16) 1_455 . . . ?
Co1 O1 C2 O6 0.14(19) 1_455 . . . ?
Co1 O1 C2 C1 -175.50(16) 1_455 . . . ?
Co1 O3 C5 O5 -12.5(4) . . . . ?
Co1 O3 C5 C4 165.80(14) . . . . ?
Co1 N1 C10 C9 -174.8(2) . . . . ?
Co1 N1 C6 C7 175.5(2) . . . . ?
O3 C5 C4 C1 145.0(2) . . . . ?
O3 C5 C4 C3 -38.4(3) . . . 3_566 ?
O5 C5 C4 C1 -36.5(3) . . . . ?
O5 C5 C4 C3 140.1(2) . . . 3_566 ?
N1 C10 C9 C8 -1.0(4) . . . . ?
N1 C6 C7 C8 -0.4(4) . . . . ?
C2 C1 C4 C5 -7.4(3) . . . . ?
C2 C1 C4 C3 176.06(19) . . . 3_566 ?
C2 C1 C3 C4 -176.24(19) . . . 3_566 ?
C4 C1 C2 O6 106.3(2) . . . . ?
C4 C1 C2 O1 -78.0(3) . . . . ?
C4 C1 C3 C4 0.3(3) . . . 3_566 ?
C3 C1 C2 O6 -77.2(3) . . . . ?
C3 C1 C2 O1 98.4(2) . . . . ?
C3 C1 C4 C5 176.24(19) . . . . ?
C3 C1 C4 C3 -0.3(3) . . . 3_566 ?
C10 N1 C6 C7 0.7(4) . . . . ?
C6 N1 C10 C9 0.0(4) . . . . ?
C9 C8 C7 C6 -0.6(4) . . . . ?
C9 C8 C11 C11 -156.5(4) . . . 3_867 ?
C7 C8 C9 C10 1.2(4) . . . . ?
C7 C8 C11 C11 22.3(5) . . . 3_867 ?
C11 C8 C9 C10 -179.9(3) . . . . ?
C11 C8 C7 C6 -179.4(3) . . . . ?
