#------------------------------------------------------------------------------
#$Date: 2019-11-17 14:32:55 +0200 (Sun, 17 Nov 2019) $
#$Revision: 230519 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/72/7057259.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_7057259
loop_
_publ_author_name
'Hou, Xiangyang'
'Wang, Xiao'
'Liu, Xiangyu'
'Wang, Jijiang'
'Tang, Long'
'Ju, Ping'
_publ_section_title
;
 Fine-tuning the effects of auxiliary ligands on two trigonal-bipyramid
 cobalt(ii) complexes exhibiting field-induced slow magnetic relaxation
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              8583
_journal_paper_doi               10.1039/C8NJ01201F
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C7 H7 Co N O6'
_chemical_formula_weight         260.07
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-04-02 deposited with the CCDC.
2018-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.172(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.873(8)
_cell_length_b                   11.983(10)
_cell_length_c                   7.366(8)
_cell_measurement_reflns_used    2392
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.73
_cell_volume                     841.1(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2092
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.480
_diffrn_reflns_theta_min         2.731
_exptl_absorpt_coefficient_mu    2.049
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Face indexing'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_description       plates
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.296
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         784
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0227
_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)+(0.0230P)²+1.6471P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0601
_reflns_Friedel_coverage         0.000
_reflns_number_gt                771
_reflns_number_total             784
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8nj01201f2.cif
_cod_data_source_block           t
_cod_depositor_comments
'Adding full bibliography for 7057259--7057260.cif.'
_cod_database_code               7057259
_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.
;
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
Co1 Co 1.0000 0.66134(3) 0.2500 0.01574(15) Uani 1 2 d S T P
O1 O 0.86213(15) 0.52337(13) 0.2583(2) 0.0265(4) Uani 1 1 d . . .
O2 O 0.74787(17) 0.68053(12) 0.2009(3) 0.0288(4) Uani 1 1 d . . .
O3 O 0.96284(17) 0.67009(12) -0.0396(2) 0.0246(4) Uani 1 1 d D . .
N1 N 0.5000 0.34421(18) 0.2500 0.0162(5) Uani 1 2 d S T P
C1 C 0.7500(2) 0.57780(17) 0.2313(3) 0.0182(4) Uani 1 1 d . . .
C2 C 0.61824(19) 0.51827(16) 0.2377(3) 0.0161(4) Uani 1 1 d . . .
C3 C 0.61231(19) 0.40255(17) 0.2334(3) 0.0168(4) Uani 1 1 d . . .
H3 H 0.6900 0.3634 0.2182 0.020 Uiso 1 1 calc R U .
C4 C 0.5000 0.5772(2) 0.2500 0.0170(6) Uani 1 2 d S T P
H4 H 0.5000 0.6549 0.2500 0.020 Uiso 1 2 calc R U P
H3B H 0.901(2) 0.7192(16) -0.087(3) 0.020 Uiso 1 1 d D U .
H3A H 0.940(2) 0.6088(12) -0.096(3) 0.020 Uiso 1 1 d D 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
O3 Co1 O3 174.19(8) . 2_755
O3 Co1 O1 97.19(6) . .
O3 Co1 O1 87.29(6) 2_755 .
O3 Co1 O1 87.29(6) . 2_755
O3 Co1 O1 97.19(6) 2_755 2_755
O1 Co1 O1 79.64(10) . 2_755
O3 Co1 N1 87.10(4) . 3
O3 Co1 N1 87.10(4) 2_755 3
O1 Co1 N1 140.18(5) . 3
O1 Co1 N1 140.18(5) 2_755 3
C1 O1 Co1 97.74(14) . .
Co1 O3 H3B 112.0(17) . .
Co1 O3 H3A 114.7(17) . .
H3B O3 H3A 109(2) . .
C3 N1 C3 117.3(2) 2_655 .
C3 N1 Co1 121.36(12) 2_655 3_445
C3 N1 Co1 121.36(12) . 3_445
O2 C1 O1 120.82(18) . .
O2 C1 C2 120.11(18) . .
O1 C1 C2 119.06(18) . .
C4 C2 C3 118.62(18) . .
C4 C2 C1 120.85(19) . .
C3 C2 C1 120.53(17) . .
N1 C3 C2 123.28(18) . .
N1 C3 H3 118.4 . .
C2 C3 H3 118.4 . .
C2 C4 C2 118.8(3) 2_655 .
C2 C4 H4 120.6 2_655 .
C2 C4 H4 120.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O3 2.071(3) .
Co1 O3 2.071(3) 2_755
Co1 O1 2.152(2) .
Co1 O1 2.152(2) 2_755
Co1 N1 2.191(3) 3
O1 C1 1.255(3) .
O2 C1 1.250(3) .
O3 H3B 0.853(10) .
O3 H3A 0.846(10) .
N1 C3 1.343(2) 2_655
N1 C3 1.343(2) .
N1 Co1 2.191(3) 3_445
C1 C2 1.495(3) .
C2 C4 1.388(2) .
C2 C3 1.388(3) .
C3 H3 0.9300 .
C4 C2 1.388(2) 2_655
C4 H4 0.9300 .
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_4
Co1 O1 C1 O2 3.6(2) . .
Co1 O1 C1 C2 -175.84(15) . .
O2 C1 C2 C4 -13.7(3) . .
O1 C1 C2 C4 165.77(17) . .
O2 C1 C2 C3 167.01(19) . .
O1 C1 C2 C3 -13.6(3) . .
C3 N1 C3 C2 1.76(14) 2_655 .
Co1 N1 C3 C2 -178.24(14) 3_445 .
C4 C2 C3 N1 -3.5(3) . .
C1 C2 C3 N1 175.90(16) . .
C3 C2 C4 C2 1.61(13) . 2_655
C1 C2 C4 C2 -177.7(2) . 2_655
