Micro-focused X-ray diffraction characterization of high-quality [6,6]-phenyl-C61-butyric acid methyl ester single crystals without solvent impurities
Giuseppe Paterna; Anna J. Warren; Jacob Spencer; Gwyndaf Evans; Victoria Garcia Sakai; Jochen Blumberger; Franco Cacialli; Journal of Materials Chemistry C 1 (2013) 5619–5623; doi:10.1039/C3TC31075B

data_7233501
_publ_section_title
;
 Micro-focused X-ray diffraction characterization of high-quality
 [6,6]-phenyl-C61-butyric acid methyl ester single crystals without
 solvent impurities
;
_journal_name_full               'Journal of Materials Chemistry C'
_journal_page_first              5619
_journal_page_last               5623
_journal_paper_doi               10.1039/C3TC31075B
_journal_volume                  1
_journal_year                    2013
_chemical_formula_moiety         'C72 H14 O2'
_chemical_formula_sum            'C72 H14 O2'
_chemical_formula_weight         910.83
_chemical_name_common
; 
Phenyl-C61-butyric acid methyl ester'
;
_chemical_name_systematic
; 
Phenyl-C61-butyric acid methyl ester'
;
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 106.9000(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.47310(10)
_cell_length_b                   15.13760(10)
_cell_length_c                   19.00509(12)
_cell_measurement_reflns_used    18434
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.7962
_cell_measurement_theta_min      1.8100
_cell_volume                     3708.70(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,Version 1.171.36.21
;
_computing_data_collection       'GDA (www.opengda.org)'
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,Version 1.171.36.21
;
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'silicon pixel detector'
_diffrn_detector_type            'Dectris Pilatus2 6MF'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'one-circle \p diffractometer'
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I24'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.62000
_diffrn_reflns_av_R_equivalents  0.1106
_diffrn_reflns_av_sigmaI/netI    0.0518
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            43780
_diffrn_reflns_theta_full        22.80
_diffrn_reflns_theta_max         22.80
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73231
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.631
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.330
_refine_diff_density_min         -0.269
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         7504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0859P)^2^+0.8846P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1426
_refine_ls_wR_factor_ref         0.1503
_reflns_number_gt                6365
_reflns_number_total             7504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            J-Mater-Chem-C-2013-1-5619.cif
_cod_data_source_block           ucl_4
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the built-in table derived from the
CIF Core dictionary named 'cif_core.dic' version 2.4.5 last updated
on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        3708.72(4)
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7233501