Synthesis of Unstable Carbides Ag2C2n (n = 3, 4) and Characterization via Crystallographic Analysis of Their Double Salts with Silver(I) Trifluoroacetate.
Hau, Sam C. K.; Mak, Thomas C. W.; Journal of the American Chemical Society 136 (2014) 902–905; doi:10.1021/ja412095y

data_4120535
_publ_section_title
;
 Synthesis of Unstable Carbides Ag2C2n (n = 3, 4) and Characterization via
 Crystallographic Analysis of Their Double Salts with Silver(I)
 Trifluoroacetate.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              902
_journal_page_last               905
_journal_paper_doi               10.1021/ja412095y
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C60 H60 Ag15 F30 O30 S10'
_chemical_formula_weight         3769.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 129.7870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   58.133(4)
_cell_length_b                   11.8141(9)
_cell_length_c                   39.378(3)
_cell_measurement_temperature    173(2)
_cell_volume                     20782(3)
_computing_cell_refinement       SAINT(Bruker,2001)
_computing_data_collection       APEX2(Bruker,2003)
_computing_data_reduction        APEX2(Bruker,2003)
_computing_molecular_graphics    DIAMOND
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD diffractometer'
_diffrn_measurement_method       '\f and \w scan'
_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  0.1329
_diffrn_reflns_av_sigmaI/netI    0.0706
_diffrn_reflns_limit_h_max       69
_diffrn_reflns_limit_h_min       -68
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            168351
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         0.91
_exptl_absorpt_coefficient_mu    3.078
_exptl_absorpt_correction_T_max  0.3723
_exptl_absorpt_correction_T_min  0.3723
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    2.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             14360
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         2.675
_refine_diff_density_min         -2.914
_refine_diff_density_rms         0.311
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1342
_refine_ls_number_reflns         18835
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0803
_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^)+(0.1179P)^2^+370.7807P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2084
_refine_ls_wR_factor_ref         0.2266
_reflns_number_gt                14831
_reflns_number_total             18835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja412095y_si_002.cif
_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/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 
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4120535