High-nuclear heterometallic oxime clusters assembled from triangular subunits: solvothermal syntheses, crystal structures and magnetic properties.
Dong, Hui-Ming; Zhang, Zhi-Chao; Li, Hai-Yan; Liu, Zhong-Yi; Yang, En-Cui; Zhao, Xiao-Jun; Dalton transactions (Cambridge, England : 2003) 47 (2017) 169–179; doi:10.1039/c7dt03692b

data_7044813
_publ_section_title
;
 High-nuclear heterometallic oxime clusters assembled from triangular
 subunits: solvothermal syntheses, crystal structures and magnetic
 properties.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              169
_journal_page_last               179
_journal_paper_doi               10.1039/c7dt03692b
_journal_volume                  47
_journal_year                    2017
_chemical_formula_sum            'C99.5 H129.5 Dy5 N67.5 Ni10 O44.5'
_chemical_formula_weight         4382.80
_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'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-03-10 deposited with the CCDC.
2017-11-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.8810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.4358(15)
_cell_length_b                   26.7521(16)
_cell_length_c                   21.9223(13)
_cell_measurement_reflns_used    9994
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.41
_cell_volume                     15225.0(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43512
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         1.093
_exptl_absorpt_coefficient_mu    3.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_density_meas      ?
_exptl_crystal_description       block
_exptl_crystal_F_000             8660
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_exptl_transmission_factor_max   0.587
_exptl_transmission_factor_min   0.554
_platon_squeeze_details
; The unit cell contains 20 nitrate ions, 26 methanol molecules 
and 26 acetonitrile molecules which have been treated as a diffuse 
contribution to the overall scattering without specific atom 
positions by SQUEEZE/PLATON. 
;
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.833
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     805
_refine_ls_number_reflns         13434
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0322
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0456P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0839
_refine_ls_wR_factor_ref         0.0874
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10943
_reflns_number_total             13434
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt03692b2.cif
_cod_data_source_block           3
_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 

 Adding full bibliography for 7044813--7044818.cif.
;
_cod_original_formula_sum        'C99.50 H129.50 Dy5 N67.50 Ni10 O44.50'
_cod_database_code               7044813
_shelx_estimated_absorpt_t_min   0.554
_shelx_estimated_absorpt_t_max   0.587
_shelxl_version_number           2013-2
_shelx_res_checksum              37502