Generation of a solid Brønsted acid site in a chiral framework.
Ingleson, Michael J; Barrio, Jorge Perez; Bacsa, John; Dickinson, Calum; Park, Hyunsoo; Rosseinsky, Matthew J; Chemical communications (Cambridge, England)  (2008) 1287–1289; doi:10.1039/b718443c

data_7102965
_publ_section_title
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 Generation of a solid Br\/onsted acid site in a chiral framework.
;
_journal_issue                   11
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1287
_journal_page_last               1289
_journal_paper_doi               10.1039/b718443c
_journal_year                    2008
_chemical_absolute_configuration rmad
_chemical_formula_sum            'C22 H32 Cu2 N4 O12'
_chemical_formula_weight         671.60
_chemical_name_common            c832
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
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2007-09-27 # Formatted by J.Bacsa

2008-01-06 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 91.713(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.6444(9)
_cell_length_b                   24.942(3)
_cell_length_c                   7.9004(11)
_cell_measurement_reflns_used    2614
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      0.956
_cell_volume                     1308.7(3)
_computing_cell_refinement       'SAINT v6.45a (Bruker, 2005)'
_computing_data_collection       'SMART v.5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT v6.45a (Bruker, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.953
_diffrn_measured_fraction_theta_max 0.953
_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  0.0208
_diffrn_reflns_av_sigmaI/netI    0.0658
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6223
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    1.697
_exptl_absorpt_correction_T_max  0.9140
_exptl_absorpt_correction_T_min  0.7278
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
A combination of a face-indexed absorption and a multi-scan correction (in
SADABS) was applied.
The crystal faces were indexed, and distances measured using the SMART
software.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'pinacoidal with 6 faces'
_exptl_crystal_F_000             692
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
Two solvent accessible regions are present in the unit cell.
TG and CHN analysis indicate 2 water molecule and
2 methanol molecule for each formula unit.
The SQUEEZE routine in PLATON (Spek, 2003) was used to remove the
contributions of the disordered solvent from diffraction intensities in
order to improve the refinement of ordered parts within the structure.
A total of 46 electrons for each void volume of 163 \%A^3^ was
equated to approximately 1 methanol molecule and 1 water molecule, or
50 per electrons per asymmetric unit.

An independent refinement on the data not treated by SQUEEZE showed electron
density that corresponded to water and methanol, but not ethenebipyridine.

;
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.920
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5161
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0428P)^2^+1.8299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1118
_refine_ls_wR_factor_ref         0.1141
_reflns_number_gt                4806
_reflns_number_total             5161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b718443c.txt
_cod_data_source_block           c832msvr
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7102965