Synthesis and structure of cationic guanidinate-bridged bimetallic {Li(7)M} cubes (M = Mn, Co, Zn) with inverse crown counter anions.
Woodruff, Daniel; Bodensteiner, Michael; Sells, Daniel O.; Winpenny, Richard E. P.; Layfield, Richard A.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 10918–10923; doi:10.1039/c1dt10999e

data_7017053
_publ_section_title
;
 Synthesis and structure of cationic guanidinate-bridged bimetallic
 {Li(7)M} cubes (M = Mn, Co, Zn) with inverse crown counter anions.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10918
_journal_page_last               10923
_journal_paper_doi               10.1039/c1dt10999e
_journal_volume                  40
_journal_year                    2011
_chemical_compound_source        'see text'
_chemical_formula_moiety
'C42 H72 Li7 Mn N18 O, C30 H90 Cl Li5 N5 Si10, 2(C7 H8)'
_chemical_formula_sum            'C86 H178 Cl Li12 Mn N23 O Si10'
_chemical_formula_weight         1988.96
_chemical_name_systematic        ?
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'May 13 10:57:32 2011'
_audit_creation_method           'PLATON <TABLE ACC> option'
_cell_angle_alpha                90
_cell_angle_beta                 105.769(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1096(12)
_cell_length_b                   24.4769(15)
_cell_length_c                   24.9736(17)
_cell_measurement_reflns_used    6420
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      23.9788
_cell_measurement_theta_min      2.9161
_cell_volume                     11829.9(13)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
;
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector_area_resol_mean 8.3367
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_device_type  'Xcalibur, Sapphire2, large Be window'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0906
_diffrn_reflns_av_sigmaI/netI    0.1765
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21119
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        21.00
_diffrn_reflns_theta_max         24.04
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.284
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66492
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov 6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4260
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.273
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         7584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1783
_refine_ls_R_factor_gt           0.0857
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0952P)^2^+17.5420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1979
_refine_ls_wR_factor_ref         0.2215
_reflns_number_gt                3705
_reflns_number_total             7584
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c1dt10999e.txt
_cod_data_source_block           oral145
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7017053