Synthesis, magnetism and spectral studies of six defective dicubane tetranuclear {M4O6} (M = Ni(II), Co(II), Zn(II)) and three trinuclear Cd(II) complexes with polydentate Schiff base ligands.
Jiang, Lin; Zhang, Dong-Yan; Suo, Jing-Jing; Gu, Wen; Tian, Jin-Lei; Liu, Xin; Yan, Shi-Ping; Dalton transactions (Cambridge, England : 2003) 45 (2016) 10233–10248; doi:10.1039/c6dt00380j

data_7702065
_publ_section_title
;
 Synthesis, magnetism and spectral studies of six defective dicubane
 tetranuclear {M4O6} (M = Ni(II), Co(II), Zn(II)) and three trinuclear
 Cd(II) complexes with polydentate Schiff base ligands.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10233
_journal_page_last               10248
_journal_paper_doi               10.1039/c6dt00380j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C19 H21 N5 Ni2 O6, 3(C3 H7 N O)'
_chemical_formula_sum            'C28 H42 N8 Ni2 O9'
_chemical_formula_weight         752.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-11-24
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2015-12-21 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                66.12(3)
_cell_angle_beta                 80.13(3)
_cell_angle_gamma                79.10(3)
_cell_formula_units_Z            2
_cell_length_a                   11.220(2)
_cell_length_b                   12.342(3)
_cell_length_c                   13.322(3)
_cell_measurement_reflns_used    4666
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8944
_cell_measurement_theta_min      2.3835
_cell_volume                     1647.2(7)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_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
;
????
;
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
scan:
	Number of images: 180
	           Slice: -110.0000 - 70.0000
	     Image width: 1.0000
	        Exp time: 4.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 45.0089
	          2theta: -19.9118
scan:
	Number of images: 150
	           Slice: -110.0000 - 40.0000
	     Image width: 1.0000
	        Exp time: 4.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 45.0089
	          2theta: -19.9118
scan:
	Number of images: 100
	           Slice: -110.0000 - -10.0000
	     Image width: 1.0000
	        Exp time: 4.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 45.0089
	          2theta: -19.9118
;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.0360
_diffrn_orient_matrix_UB_12      -0.0758
_diffrn_orient_matrix_UB_13      -0.0359
_diffrn_orient_matrix_UB_21      -0.0856
_diffrn_orient_matrix_UB_22      -0.0172
_diffrn_orient_matrix_UB_23      -0.0194
_diffrn_orient_matrix_UB_31      0.0348
_diffrn_orient_matrix_UB_32      0.0524
_diffrn_orient_matrix_UB_33      -0.0535
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16738
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.903
_diffrn_reflns_theta_min         1.681
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.207
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8738
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_description       Prism
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.795
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         7728
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0576
_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^)+(0.1140P)^2^+1.4270P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1672
_refine_ls_wR_factor_ref         0.1824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5540
_reflns_number_total             7728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00380j2.cif
_cod_data_source_block           nide
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_database_code               7702065
_shelxl_version_number           2013-4
_diffrn_number_total             7730
_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 O(H,H) groups
2. Rigid bond restraints
 N3, N4, N5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
3. Uiso/Uaniso restraints and constraints
N3 \\sim N4 \\sim N5: within 2A with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(N5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Rotating group:
 O6(H6A,H6B)
4.b Ternary CH refined with riding coordinates:
 C10(H10)
4.c Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B)
4.d Aromatic/amide H refined with riding coordinates:
 C8(H8), C16(H16), C12(H12), C4(H4), C5(H5), C6(H6), C14(H14), C15(H15),
 C19(H19), C23(H23), C25(H25)
4.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C38(H38A,H38B,H38C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C22(H22A,H22B,H22C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C24(H24A,
 H24B,H24C)
;
_shelx_res_checksum              24889
_olex2_submission_special_instructions 'No special instructions were received'