Synthesis and Single-Crystal Structure Analysis of [Ba(NH3)7]C60.NH3
Klaus Himmel; Martin Jansen; Inorganic Chemistry 37 (1998) 3437–3439; doi:10.1021/ic9715512

data_4322862
_publ_contact_author
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     Jansen, Martin
      Institut f. Anorg. Chemie der Universit\"at Bonn
      Gerhard-Domagk-Str. 1
      D-53121 Bonn
      Germany
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_publ_contact_author_email       mjansen@snchemie2.chemie.uni-bonn.de
_publ_contact_author_fax         '228 73 5660'
_publ_contact_author_phone       '228 73 2708'
_publ_section_title
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 Synthesis and Single-Crystal Structure Analysis of [Ba(NH3)7]C60.NH3
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3437
_journal_page_last               3439
_journal_paper_doi               10.1021/ic9715512
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         '(Ba H21 N7 +) (C60 2-) x NH3'
_chemical_formula_sum            'C60 H24 Ba N8'
_chemical_formula_weight         994.21
_chemical_name_systematic
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 barium heptaammine fulleride ammonia (1/1)
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_space_group_IT_number           160
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3 -2"'
_symmetry_space_group_name_H-M   'R 3 m :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   12.223(2)
_cell_length_b                   12.223(2)
_cell_length_c                   21.461(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      7.91
_cell_volume                     2776.7(10)
_computing_cell_refinement       'CELDIM (CAD4 software)'
_computing_data_collection       'CAD4 software version 5.0'
_computing_data_reduction        'CADSHEL (J.Kopf, H.C. Ruebke, Hamburg)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       '\w/\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7256
_diffrn_reflns_theta_max         26.95
_diffrn_reflns_theta_min         2.15
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.863
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.38(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1279
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.067
_refine_ls_restrained_S_obs      1.064
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_obs          0.0226
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+4.3990P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0558
_refine_ls_wR_factor_obs         0.0553
_reflns_number_observed          1267
_reflns_number_total             1279
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715512.cif
_cod_data_source_block           batw
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+4.3990P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+4.3990P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_sg_symbol_H-M      'R 3 m'
_cod_database_code               4322862