Synthesis and characterization of [ru@ge12](3-): an endohedral 3-connected cluster.
Espinoza-Quintero, Gabriela; Duckworth, Jack C. A.; Myers, William K.; McGrady, John E.; Goicoechea, Jose M.; Journal of the American Chemical Society 136 (2014) 1210–1213; doi:10.1021/ja411280v

data_4120481
_publ_contact_author
;
 Dr. J. M. Goicoechea           
 Chemistry Research Laboratory
 University of Oxford
 Mansfield Road
 Oxford
 OX1 3TA
 UK
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_publ_section_title
;
 Synthesis and characterization of [ru@ge12](3-): an endohedral
 3-connected cluster.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1210
_journal_page_last               1213
_journal_paper_doi               10.1021/ja411280v
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         '3(C18 H36 K N2 O6), Ge12 Ru, 4(C5 H5 N)'
_chemical_formula_sum            'C74 H128 Ge12 K3 N10 O18 Ru'
_chemical_formula_weight         2535.31
_chemical_name_systematic
;
[K(2,2,2-crypt)]3[Ru@Ge12]*4py
;
_space_group_IT_number           4
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_cell_formula_units_Z            2
_cell_length_a                   14.14240(10)
_cell_length_b                   26.0428(2)
_cell_length_c                   14.26840(10)
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_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      76.2445
_cell_measurement_theta_min      3.2495
_cell_volume                     5004.88(7)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
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_computing_molecular_graphics    'WinGX (Farrugia, 2005)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  area
_diffrn_measurement_method       'omega scans'
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_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
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_diffrn_reflns_limit_l_min       -17
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_diffrn_reflns_theta_full        76.43
_diffrn_reflns_theta_max         76.43
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_exptl_absorpt_coefficient_mu    6.790
_exptl_absorpt_correction_T_max  0.7729
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.8 (release 07-03-2011 CrysAlis171 .NET)
(compiled Mar  7 2011,18:06:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.682
_exptl_crystal_density_meas      ?
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_exptl_crystal_description       plate
_exptl_crystal_F_000             2542
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.478
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1161
_refine_ls_number_reflns         19737
_refine_ls_number_restraints     115
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0615
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1120P)^2^+3.4347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1552
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                18305
_reflns_number_total             19737
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja411280v_si_002.cif
_cod_data_source_block           1
_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/current/ACS/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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        5004.88(6)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               4120481