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_7702069
_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 H46 Br4 N4 Ni4 O14, 2(C H3 O), O'
_chemical_formula_sum            'C44 H54 Br4 N4 Ni4 O17'
_chemical_formula_weight         1465.39
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-12-21 deposited with the CCDC.
2016-05-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 111.483(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.937(10)
_cell_length_b                   11.757(4)
_cell_length_c                   16.933(6)
_cell_measurement_reflns_used    4527
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     5175(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -120.0000 - 60.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 0.0000
	             XTD: 49.8438
	          2theta: -30.1104
scan:
	Number of images: 300
	           Slice: -120.0000 - 30.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 90.0000
	             XTD: 49.8438
	          2theta: -30.1104
scan:
	Number of images: 200
	           Slice: -120.0000 - -20.0000
	     Image width: 0.5000
	        Exp time: 2.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 49.8438
	          2theta: -30.1104
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Rigaku Pilatus 200K'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      0.023323
_diffrn_orient_matrix_UB_12      0.018805
_diffrn_orient_matrix_UB_13      0.024128
_diffrn_orient_matrix_UB_21      0.025974
_diffrn_orient_matrix_UB_22      0.049771
_diffrn_orient_matrix_UB_23      -0.063898
_diffrn_orient_matrix_UB_31      -0.029270
_diffrn_orient_matrix_UB_32      0.049572
_diffrn_orient_matrix_UB_33      0.026714
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20917
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         3.13
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.595
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.809
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.881
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2936
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.068
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.271
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5947
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.271
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1706
_refine_ls_wR_factor_ref         0.1757
_reflns_number_gt                4957
_reflns_number_total             5947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6dt00380j2.cif
_cod_data_source_block           ni
_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               7702069
_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
2. Others
 Fixed Sof: Br4(0.5) Br1(0.5)
3.a Ternary CH refined with riding coordinates:
 C15(H15)
3.b Secondary CH2 refined with riding coordinates:
 C16(H16a,H16b), C29(H29a,H29b)
3.c Aromatic/amide H refined with riding coordinates:
 C20(H20), C24(H24), C26(H26), C28(H28), C32(H32), C34(H34)
3.d Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C17(H17a,H17b,H17c), C23(H23a,H23b,H23c), C33(H33a,H33b,
 H33c), C46(H46a,H46b,H46c)
;
_olex2_submission_special_instructions 'No special instructions were received'