Coligand effects on the architectures and magnetic properties of octahedral cobalt(ii) complexes with easy-axis magnetic anisotropy
Wu, Yuewei; Xi, Jing; Yang, Jinhui; Song, Weiming; Luo, Shuchang; Wang, Zheng; Liu, Xiangyu; CrystEngComm 22 (2020) 2297–2303; doi:10.1039/C9CE01871A

data_7239972
_publ_section_title
;
 Coligand effects on the architectures and magnetic properties of
 octahedral cobalt(ii) complexes with easy-axis magnetic anisotropy
;
_journal_issue                   13
_journal_name_full               CrystEngComm
_journal_page_first              2297
_journal_page_last               2303
_journal_paper_doi               10.1039/C9CE01871A
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C24 H20 Co N18, H2 O'
_chemical_formula_sum            'C24 H22 Co N18 O'
_chemical_formula_weight         637.52
_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             2018-01-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-11-04 deposited with the CCDC.	2020-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.327(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1218(7)
_cell_length_b                   14.2515(7)
_cell_length_c                   14.6292(8)
_cell_measurement_reflns_used    4005
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.1100
_cell_measurement_theta_min      2.7560
_cell_volume                     2672.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -40.00  62.00   1.00   18.00    --  -11.59  57.00-120.00  102
  2  \w     -5.00  85.00   1.00   18.00    --   11.74  77.00 120.00   90
  3  \w    -20.00   5.00   1.00   18.00    --  -11.59 -99.00 -30.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0151246000
_diffrn_orient_matrix_UB_12      -0.0416294000
_diffrn_orient_matrix_UB_13      0.0259303000
_diffrn_orient_matrix_UB_21      -0.0465978000
_diffrn_orient_matrix_UB_22      -0.0222781000
_diffrn_orient_matrix_UB_23      -0.0235838000
_diffrn_orient_matrix_UB_31      0.0257222000
_diffrn_orient_matrix_UB_32      -0.0157733000
_diffrn_orient_matrix_UB_33      -0.0351261000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15181
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.527
_diffrn_reflns_theta_min         2.018
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.701
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         6389
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0595
_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/[\s^2^(Fo^2^)+(0.0480P)^2^+2.1040P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1386
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4557
_reflns_number_total             6389
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ce01871a9.cif
_cod_data_source_block           pre_xh_9
_cod_depositor_comments
;Adding full bibliography for 7239971--7239972.cif.

 Adding full bibliography for 7239971--7239972.cif.
;
_cod_database_code               7239972
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.927
_shelx_estimated_absorpt_t_min   0.914
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Rigid bond restraints
 N13, N14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
N13 \\sim N14: within 2A with sigma of 0.002 and sigma for terminal atoms of
0.004
4.a Free rotating group:
 O1(H1A,H1B)
4.b Rotating group:
 N3(H3A,H3B), N11(H11A,H11B)
4.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C10(H10), C9(H9), C3(H3), C6(H6),
 C21(H21), C5(H5), C22(H22), C16(H16), C4(H4), C15(H15), C23(H23), C24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.282
_oxdiff_exptl_absorpt_empirical_full_min 0.837