Encapsulation of molecular Na2SiF6 by two metallacrown complexes
Lehaire, Marie-Line; Scopelliti, Rosario; Severin, Kay; Chemical Communications  (2002) 2766–; doi:10.1039/b208996c

data_7114440
_publ_section_title
;
 Encapsulation of molecular Na2SiF6 by two metallacrown complexes
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2766
_journal_paper_doi               10.1039/b208996c
_journal_year                    2002
_chemical_formula_moiety         'C90 H102 F6 N6 Na2 O12 Ru6 Si, 2(H2 O)'
_chemical_formula_sum            'C90 H106 F6 N6 Na2 O14 Ru6 Si'
_chemical_formula_weight         2290.30
_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                 109.567(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5292(10)
_cell_length_b                   29.415(3)
_cell_length_c                   13.0113(14)
_cell_measurement_reflns_used    2630
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      18.8826
_cell_measurement_theta_min      2.1829
_cell_volume                     4518.3(8)
_computing_cell_refinement       'Oxford Diffraction, CrysAlis RED'
_computing_data_collection       'Oxford Diffraction, CrysAlis CCD'
_computing_data_reduction        'Oxford Diffraction, CrysAlis RED'
_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      140(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'Oxford Diffraction, KM4CCD/SAPPHIRE'
_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  0.1487
_diffrn_reflns_av_sigmaI/netI    0.2727
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            26357
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    1.078
_exptl_absorpt_correction_T_max  0.8410
_exptl_absorpt_correction_T_min  0.5010
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
; 
(See: Walker, N. & Stuart, D. (1983) Acta Cryst. A39, 158-166) 
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2308
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.530
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.891
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     572
_refine_ls_number_reflns         7286
_refine_ls_number_restraints     415
_refine_ls_restrained_S_all      0.868
_refine_ls_R_factor_all          0.2032
_refine_ls_R_factor_gt           0.0717
_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^)+(0.0000P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0800
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                3248
_reflns_number_total             7286
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b208996c.txt
_cod_data_source_block           3
_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        4518.4(7)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7114440