1,2-[3,4-Dihydro-2-(4-methoxyphenyl)-2<i>H</i>-pyrrolo][60]fullerene Carbon Disulfide
Ramm, M.; Luger, P.; Averdung, J.; Mattay, J.; Acta Crystallographica Section C 52 (1996) 2590–2594; doi:10.1107/S0108270196009742

data_2005525
_publ_contact_author
;
      Dr. Matthias Ramm
      Freie Universit\"at Berlin
      Institut f\"ur Kristallographie
      Takustr. 6
      14195 Berlin
      Germany
;
_publ_section_title
;
 1,2-[3,4-Dihydro-2-(4-methoxyphenyl)-2<i>H</i>-pyrrolo][60]fullerene
 Carbon Disulfide
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2590
_journal_page_last               2594
_journal_paper_doi               10.1107/S0108270196009742
_journal_volume                  52
_journal_year                    1996
_chemical_formula_moiety         'C69 H9 N O, C S2'
_chemical_formula_sum            'C70 H9 N O S2'
_chemical_formula_weight         943.90
_chemical_name_systematic
;
1,2-[3,4-Dihydro-2-(5-methoxyphenyl)-2H-pyrrolo)[60]fullerene
;
_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'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.18(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.094(4)
_cell_length_b                   10.022(3)
_cell_length_c                   17.293(4)
_cell_measurement_reflns_used    61
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      36
_cell_measurement_theta_min      15
_cell_volume                     3655.8(15)
_computing_cell_refinement       'Stoe diffractometer software'
_computing_data_collection       'Stoe diffractometer software'
_computing_data_reduction        'Stoe diffractometer software'
_computing_molecular_graphics
'ORTEPII (Johnson, 1971), SCHAKAL92 (Keller, 1992)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293.0(10)
_diffrn_measurement_device       'Stoe AED'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  Ni-filter
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0125
_diffrn_reflns_av_sigmaI/netI    0.0690
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5642
_diffrn_reflns_theta_max         60.09
_diffrn_reflns_theta_min         3.30
_diffrn_standards_decay_%        1.2
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.829
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.251
_refine_ls_extinction_coef       0.00010(6)
_refine_ls_extinction_method     'SHELXL93  (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   0.881
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_hydrogen_treatment    'H atoms: see text below'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         5436
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.883
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_obs          0.0451
_refine_ls_shift/esd_max         0.007
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0779P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1211
_refine_ls_wR_factor_obs         0.1094
_reflns_number_observed          3098
_reflns_number_total             5436
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka1208.cif
_cod_data_source_block           global
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'YES' changed to 'yes' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (105
times).

'_geom_angle_publ_flag' value 'YES' changed to 'yes'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (203
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0779P)^2^] 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^)+(0.0779P)^2^]
where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2005525