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_7702061
_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         'C20 H24 Co2 N2 O7'
_chemical_formula_sum            'C20 H24 Co2 N2 O7'
_chemical_formula_weight         522.27
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-07-22
_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                90.00
_cell_angle_beta                 102.17(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.503(2)
_cell_length_b                   17.689(4)
_cell_length_c                   14.495(3)
_cell_measurement_reflns_used    5490
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.1115
_cell_measurement_theta_min      1.8415
_cell_volume                     2632.5(10)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      113.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
scan:
	Number of images: 180
	           Slice: -120.0000 - 60.0000
	     Image width: 1.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 49.9617
	          2theta: -29.9248
scan:
	Number of images: 140
	           Slice: -120.0000 - 20.0000
	     Image width: 1.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 49.9617
	          2theta: -29.9248
scan:
	Number of images: 70
	           Slice: -120.0000 - -50.0000
	     Image width: 1.0000
	        Exp time: 8.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 49.9617
	          2theta: -29.9248
;
_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      0.0337
_diffrn_orient_matrix_UB_12      -0.0436
_diffrn_orient_matrix_UB_13      0.0803
_diffrn_orient_matrix_UB_21      -0.0486
_diffrn_orient_matrix_UB_22      -0.0284
_diffrn_orient_matrix_UB_23      0.0050
_diffrn_orient_matrix_UB_31      0.0310
_diffrn_orient_matrix_UB_32      -0.0577
_diffrn_orient_matrix_UB_33      -0.0263
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1167
_diffrn_reflns_av_unetI/netI     0.0964
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16484
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.84
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           16.0000
_diffrn_source_power             0.8000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    1.296
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3311
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_platon_squeeze_details
;
;
_refine_diff_density_max         1.262
_refine_diff_density_min         -0.649
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4646
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_gt           0.0664
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1647
_refine_ls_wR_factor_ref         0.1768
_reflns_number_gt                3287
_reflns_number_total             4646
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00380j2.cif
_cod_data_source_block           code-sr
_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_original_cell_volume        2632.4(9)
_cod_database_code               7702061
_diffrn_number_total             6058
_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
 O3, Co2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Rotating group:
 O7(H7a,H7b)
3.b Ternary CH refined with riding coordinates:
 C37(H37)
3.c Secondary CH2 refined with riding coordinates:
 C14(H14a,H14b), C34(H34a,H34b)
3.d Aromatic/amide H refined with riding coordinates:
 C33(H33), C12(H12), C13(H13), C29(H29), C24(H24), C23(H23), C31(H31), C30(H30)
3.e Idealised Me refined as rotating group:
 C21(H21a,H21b,H21c), C26(H26a,H26b,H26c), C38(H38a,H38b,H38c)
;
_olex2_submission_special_instructions 'No special instructions were received'