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_7702064
_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         'C42 H52 N4 O14 Zn4, 4(C H4 O)'
_chemical_formula_sum            'C46 H68 N4 O18 Zn4'
_chemical_formula_weight         1226.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.06.20 svn.r2946 for OlexSys, GUI svn.r4855)
;
_audit_update_record
;
2015-06-23 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.21(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.212(2)
_cell_length_b                   16.600(3)
_cell_length_c                   13.056(3)
_cell_measurement_reflns_used    7895
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8984
_cell_measurement_theta_min      1.5597
_cell_volume                     2646.7(9)
_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  'olex2.refine (Bourhis et al., 2013)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.9938
_diffrn_measured_fraction_theta_max 0.9938
_diffrn_measurement_details
;
scan:
	Number of images: 180
	           Slice: -110.0000 - 70.0000
	     Image width: 1.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 49.9890
	          2theta: -19.8952
scan:
	Number of images: 150
	           Slice: -110.0000 - 40.0000
	     Image width: 1.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 49.9890
	          2theta: -19.8952
scan:
	Number of images: 80
	           Slice: -110.0000 - -30.0000
	     Image width: 1.0000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 49.9890
	          2theta: -19.8952
;
_diffrn_measurement_device
;
Saturn70 (4x4 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0231
_diffrn_orient_matrix_UB_12      0.0393
_diffrn_orient_matrix_UB_13      -0.0681
_diffrn_orient_matrix_UB_21      -0.0733
_diffrn_orient_matrix_UB_22      -0.0074
_diffrn_orient_matrix_UB_23      0.0209
_diffrn_orient_matrix_UB_31      0.0032
_diffrn_orient_matrix_UB_32      0.0525
_diffrn_orient_matrix_UB_33      0.0293
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22224
_diffrn_reflns_theta_full        25.0070
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.07
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.865
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7953
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.5391
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1275.0807
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.3933
_refine_diff_density_min         -0.4771
_refine_diff_density_rms         0.0896
_refine_ls_d_res_high            0.8406
_refine_ls_d_res_low             9.8368
_refine_ls_goodness_of_fit_ref   1.0333
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    53
_refine_ls_number_parameters     335
_refine_ls_number_reflns         4647
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.0330
_refine_ls_R_factor_all          0.0357
_refine_ls_R_factor_gt           0.0312
_refine_ls_shift/su_max          0.0003
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+1.1696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0739
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4117
_reflns_number_total             4647
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c6dt00380j2.cif
_cod_data_source_block           Znde
_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               7702064
_diffrn_number_total             11904
_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) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 Zn1-H6
 2.759927 with sigma of 0.02
 C20-H6
 1.892168 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C9(H9a,H9b), C11(H11a,H11b)
3.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C8(H8), C16(H16), C6(H6a), C4(H4), C15(H15), C14(H14), C5(H5)
3.d Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c), C1(H1a,H1b,
 H1c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c)
3.e Idealised tetrahedral OH refined as rotating group:
 O8(H8a), O9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'