Mono-, Tetra- and octanuclear transition metal complexes of in situ generated schiff base ligands containing up to 12 coordinating atoms: syntheses, structures and magnetism
Ding, Cai-Xia; Ni, Jia; Yang, Yu-Hua; Ng, Seik-Weng; Wang, Bing-Wu; Xie, Yong-Shu; CrystEngComm 14 (2012) 7312–; doi:10.1039/c2ce25966d

data_7214829
_publ_section_title
;
 Mono-, Tetra- and octanuclear transition metal complexes of in situ
 generated schiff base ligands containing up to 12 coordinating atoms:
 syntheses, structures and magnetism
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              7312
_journal_paper_doi               10.1039/c2ce25966d
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C38.5 H58 Cl N11 Ni4 O7.5 S3'
_chemical_formula_weight         1161.43
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0550(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.1068(16)
_cell_length_b                   17.4396(18)
_cell_length_c                   20.834(2)
_cell_measurement_reflns_used    3396
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.026
_cell_measurement_theta_min      2.336
_cell_volume                     5485.3(10)
_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-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0890
_diffrn_reflns_av_sigmaI/netI    0.1546
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            27130
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    1.567
_exptl_absorpt_correction_T_max  0.7446
_exptl_absorpt_correction_T_min  0.5522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2412
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.731
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     624
_refine_ls_number_reflns         9611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1957
_refine_ls_R_factor_gt           0.0699
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+19.5459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.2640
_reflns_number_gt                4041
_reflns_number_total             9611
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25966d.txt
_cod_data_source_block           090802c
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        5485.4(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_original_formula_sum        'C38.50 H58 Cl N11 Ni4 O7.50 S3'
_cod_database_code               7214829