Exceptionally slow magnetic relaxation in a mononuclear hexacoordinate Ni(ii) complex.
Titiš, Ján; Chrenková, Veronika; Rajnák, Cyril; Moncol, Ján; Valigura, Dušan; Boča, Roman; Dalton transactions (Cambridge, England : 2003) 48 (2019) 11647–11650; doi:10.1039/c9dt02159k

data_7700500
_publ_section_title
;
 Exceptionally slow magnetic relaxation in a mononuclear hexacoordinate
 Ni(ii) complex.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11647
_journal_page_last               11650
_journal_paper_doi               10.1039/c9dt02159k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C14 H18 N2 Ni O4, 2(C7 H3 N2 O6)'
_chemical_formula_sum            'C28 H24 N6 Ni O16'
_chemical_formula_weight         759.24
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-05-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-11 deposited with the CCDC.    2019-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                96.452(2)
_cell_angle_beta                 103.366(2)
_cell_angle_gamma                100.715(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9708(2)
_cell_length_b                   13.7985(4)
_cell_length_c                   14.6800(4)
_cell_measurement_reflns_used    39964
_cell_measurement_temperature    100
_cell_measurement_theta_max      71.61
_cell_measurement_theta_min      3.14
_cell_volume                     1522.94(7)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.991
_diffrn_measured_fraction_theta_max 0.971
_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  0.0214
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25529
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         71.153
_diffrn_reflns_theta_min         3.136
_diffrn_source                   'Genix3D Cu HF'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.733
_exptl_absorpt_correction_T_max  0.195
_exptl_absorpt_correction_T_min  0.057
_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            'bluish green'
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.0064(2)
_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   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         5722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0393P)^2^+1.1083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5548
_reflns_number_total             5722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt02159k2.cif
_cod_data_source_block           vch14
_cod_depositor_comments          'Adding full bibliography for 7700500.cif.'
_cod_database_code               7700500
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.702
_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) groups
2.a Riding coordinates:
 O1(H1), O2(H2), O3(H3), O4(H4)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C7(H7A,H7B), C8(H8A,H8B), C14(H14A,H14B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4A), C5(H5), C10(H10), C11(H11), C12(H12), C17(H17), C19(H19),
 C21(H21), C24(H24), C26(H26), C28(H28)
;
_shelx_res_checksum              16069
_olex2_submission_special_instructions 'No special instructions were received'