Effect of the distant substituent on the slow magnetic relaxation of the mononuclear Co(ii) complex with pincer-type ligands.
Rajnák, Cyril; Titiš, Ján; Moncol', Ján; Boča, Roman; Dalton transactions (Cambridge, England : 2003) 49 (2020) 4206–4210; doi:10.1039/d0dt00096e

data_7704276
_publ_section_title
;
 Effect of the distant substituent on the slow magnetic relaxation of the
 mononuclear Co(ii) complex with pincer-type ligands.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4206
_journal_page_last               4210
_journal_paper_doi               10.1039/d0dt00096e
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C14 H18 N2 O4 Zn, 2(C8 H5 N2 O6)'
_chemical_formula_sum            'C30 H28 N6 O16 Zn'
_chemical_formula_weight         793.95
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-05 deposited with the CCDC.	2020-03-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.163(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.3034(9)
_cell_length_b                   16.8405(8)
_cell_length_c                   14.4655(6)
_cell_measurement_reflns_used    27215
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.76
_cell_measurement_theta_min      3.10
_cell_volume                     6525.4(5)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.150.0 (STOE, 2018)
;
_computing_data_reduction
;
X-Area Integrate 1.73.1.0 (STOE, 2018)
X-Area LANA 1.73.2.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.84, Darmstadt 2018
;
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Pilatus3R 300K'
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS3R 300K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'Stoe StadiVari'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_collimation    '0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            35121
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.909
_diffrn_reflns_theta_min         3.100
_diffrn_source                   'Genix3D Cu HF'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  0.657
_exptl_absorpt_correction_T_min  0.218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, J. Koziskova, F. Hahn, J. Richter, J. Kozisek, 
Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       prism
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.101
_refine_ls_extinction_coef       0.000190(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         6207
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0700
_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^)+(0.0359P)^2^+79.4458P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1581
_refine_ls_wR_factor_ref         0.1687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4682
_reflns_number_total             6207
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt00096e2.cif
_cod_data_source_block           3
_cod_database_code               7704276
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.784
_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 C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 C26-N5A \\sim C26-N5B \\sim C18-N3A \\sim C18-N3B
 with sigma of 0.005
 N5A-O13A \\sim N5B-O13B \\sim N5A-O14A \\sim N5B-O14B
 with sigma of 0.005
 N6-O15A \\sim N6-O15B \\sim N6-O16A \\sim N6-O16B
 with sigma of 0.005
 N3A-O9A \\sim N3A-O10A \\sim N3B-O9B \\sim N3B-O10B
 with sigma of 0.005
 O13A-O14A \\sim O13B-O14B \\sim O15A-O16A \\sim O15B-O16B
 with sigma of 0.01
 O9A-O10A \\sim O9B-O10B
 with sigma of 0.01
 C26-O13A \\sim C26-O13B \\sim C26-O14A \\sim C26-O14B
 with sigma of 0.01
 C28-O15A \\sim C28-O15B \\sim C28-O16A \\sim C28-O16B
 with sigma of 0.01
 C18-O9A \\sim C18-O10A \\sim C18-O9B \\sim C18-O10B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O13A) = Uanis(O14A)
Uanis(O13B) = Uanis(O14B)
Uanis(O15B) = Uanis(O16B)
Uanis(O15A) = Uanis(O16A)
Uanis(N5A) = Uanis(N5B)
Uanis(N3A) = Uanis(N3B)
Uanis(O10A) = Uanis(O10B)
Uanis(O9A) = Uanis(O9B)
4. Rigid body (RIGU) restrains
 O9A, O10A, N3A, O13A, O14A, O15A, O16A, O9B, O10B, N3B, O13B, O14B, O15B,
 O16B, N5A, N5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O13B)=Sof(O14B)=Sof(N5B)=1-FVAR(1)
 Sof(O13A)=Sof(O14A)=Sof(N5A)=FVAR(1)
 Sof(O15B)=Sof(O16B)=1-FVAR(2)
 Sof(O15A)=Sof(O16A)=FVAR(2)
 Sof(O9B)=Sof(O10B)=Sof(N3B)=1-FVAR(3)
 Sof(O9A)=Sof(O10A)=Sof(N3A)=FVAR(3)
 Fixed Sof: H30A(0.5) H30B(0.5) H30C(0.5) H30D(0.5) H30E(0.5) H30F(0.5)
6.a Riding coordinates:
 O1(H1), O2(H2), O3(H3), O4(H4)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C8(H8A,H8B), C14(H14A,H14B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C5(H5), C10(H10), C11(H11), C12(H12), C17(H17), C21(H21),
 C25(H25), C29(H29)
6.d Disordered Me refined with riding coordinates:
 C30(H30A,H30B,H30C,H30D,H30E,H30F)
6.e Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C)
;
_shelx_res_checksum              86885
_olex2_submission_special_instructions 'No special instructions were received'