A cobalt(ii) chain based on pymca generated in situ from the hydrolysis of 2-cyanopyrimidine: spin canting and magnetic relaxation
Zhang, Jie; Zhao, Qian-Nan; Yang, Feng; Yin, Lei; Li, Miao-Miao; Wang, Zhenxing; Ouyang, Zhongwen; Xia, Zheng-Cai; Hu, Tuo-Ping; RSC Advances 9 (2019) 31115–; doi:10.1039/C9RA05354A

data_7234317
_publ_section_title
;
 A cobalt(ii) chain based on pymca generated in situ from the hydrolysis
 of 2-cyanopyrimidine: spin canting and magnetic relaxation
;
_journal_issue                   53
_journal_name_full               'RSC Advances'
_journal_page_first              31115
_journal_paper_doi               10.1039/C9RA05354A
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C10 H14 Co2 N4 O8, O4 S, 2(H2 O)'
_chemical_formula_sum            'C10 H18 Co2 N4 O14 S'
_chemical_formula_weight         568.20
_space_group_crystal_system      tetragonal
_space_group_IT_number           114
_space_group_name_Hall           'P -4 2n'
_space_group_name_H-M_alt        'P -4 21 c'
_symmetry_space_group_name_Hall  'P -4 2n'
_symmetry_space_group_name_H-M   'P -4 21 c'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-09-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-02 deposited with the CCDC.    2019-09-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5941(13)
_cell_length_b                   9.5941(13)
_cell_length_c                   20.329(3)
_cell_measurement_reflns_used    3740
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.94
_cell_measurement_theta_min      2.35
_cell_volume                     1871.2(5)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SAINT (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13936
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.419
_diffrn_reflns_theta_min         2.347
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.9805
_exptl_absorpt_correction_T_min  0.7174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SABABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.017
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.194
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         2098
_refine_ls_number_restraints     131
_refine_ls_restrained_S_all      1.162
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0557
_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/[\s^2^(Fo^2^)+(0.0158P)^2^+9.1256P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1181
_refine_ls_wR_factor_ref         0.1205
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                1926
_reflns_number_total             2098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra05354a2.cif
_cod_data_source_block           20171012zqn2_0m_b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_original_cell_volume        1871.2(6)
_cod_database_code               7234317
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details   none
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.80(5)
 0.20(5)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
3. Restrained distances
 H2A-H2B
 1.38 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C2) \\sim
Ueq, Uanis(N3) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Rigid body (RIGU) restrains
 Co1, Co2, O2, O5, O6, N3, N4, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O10(H10A,H10B)
6.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4)
;
_shelx_res_checksum              29913
_olex2_submission_special_instructions 'No special instructions were received'