Field Supported Slow Magnetic Relaxation in a Mononuclear Cu(II) Complex.
Boča, Roman; Rajnák, Cyril; Titiš, Ján; Valigura, Dušan; Inorganic chemistry 56 (2017) 1478–1482; doi:10.1021/acs.inorgchem.6b02535

data_4345497
_publ_section_title
;
 Field Supported Slow Magnetic Relaxation in a Mononuclear Cu(II) Complex.
;
_journal_issue                   3
_journal_name_full               'Inorganic chemistry'
_journal_page_first              1478
_journal_page_last               1482
_journal_paper_doi               10.1021/acs.inorgchem.6b02535
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C14 H12 Cu N2 O6, 0.5(H2 O)'
_chemical_formula_sum            'C14 H13 Cu N2 O6.5'
_chemical_formula_weight         376.80
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2016-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 102.904(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.6646(3)
_cell_length_b                   22.9611(7)
_cell_length_c                   14.5027(5)
_cell_measurement_temperature    100
_cell_volume                     2812.43(17)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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    'SIR2011 (Burla et al., 2007)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'Stoe Stadivari with Xenocs Genix3D Cu HF'
_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  0.0256
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            61468
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         70.832
_diffrn_reflns_theta_min         3.672
_diffrn_source                   'Genix3D Cu HF'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.577
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.336
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5317
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0266
_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^)+(0.0413P)^2^+2.8511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0731
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4810
_reflns_number_total             5317
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02535_si_002.cif
_cod_data_source_block           hk45
_cod_depositor_comments
;

2020-07-06
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_moiety     '2(C14 H12 Cu N2 O6), H2 O'
_cod_original_formula_sum        'C28 H26 Cu2 N4 O13'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     753.61
_cod_database_code               4345497
_shelx_estimated_absorpt_t_max   0.783
_shelx_estimated_absorpt_t_min   0.627
_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,H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5 = O6-H6 = O11-H11A = O12-H12A
 0.84 with sigma of 0.001
3.a Riding coordinates:
 O1W(H1WA,H1WB)
3.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C14(H14A,H14B), C22(H22A,H22B), C28(H28A,H28B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5A), C10(H10), C11(H11), C12(H12), C17(H17), C18(H18),
 C19(H19), C24(H24), C25(H25), C26(H26)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'