Hydrogen bonding in calcium–trifluoromethanesulfonate–1,3-di-4-pyridylurea–methanol (1/2/2/4)
M. Barboiu; A. van der Lee; Acta Crystallographica Section C 59 (2003) m366–m368; doi:10.1107/S0108270103011454

data_2013411
_publ_section_title
;
 Hydrogen bonding in
 calcium--trifluoromethanesulfonate--1,3-di-4-pyridylurea--methanol
 (1/2/2/4)
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m366
_journal_page_last               m368
_journal_paper_doi               10.1107/S0108270103011454
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'Ca 2+, 2C F3 O3 S 1-, 2C11 H10 N4 O, 4C H4 O'
_chemical_formula_moiety         'Ca 2+, 2C F3 O3 S 1-, 2C11 H10 N4 O, 4C H4 O'
_chemical_formula_sum            'C28 H36 Ca F6 N8 O12 S2'
_chemical_formula_weight         894.84
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                98.950(10)
_cell_angle_beta                 97.140(10)
_cell_angle_gamma                94.030(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1570(10)
_cell_length_b                   9.7680(10)
_cell_length_c                   11.366(2)
_cell_measurement_reflns_used    4175
_cell_measurement_temperature    173
_cell_measurement_theta_max      23.20
_cell_measurement_theta_min      1.75
_cell_volume                     992.3(2)
_computing_cell_refinement       'Crysalis RED (Oxford Diffraction, 2002)'
_computing_data_collection       'Crysalis CCD (Oxford Diffraction, 2002)'
_computing_data_reduction        'Crysalis RED (2002)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  PLATON
_computing_structure_refinement
;
CRYSTALS (Watkin et al., 2001), SHELXL97 (Sheldrick, 1997) and
WinGX (Version 1.64.05; Farrugia, 1997)
;
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 17
_diffrn_measured_fraction_theta_full 1.00
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur CCD'
_diffrn_measurement_method       area-detector
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0300
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17908
_diffrn_reflns_reduction_process RED
_diffrn_reflns_theta_full        28.49
_diffrn_reflns_theta_max         28.49
_diffrn_reflns_theta_min         3.23
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  30
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.900
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   '(Schwarzenbach & Flack, 1991)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.497
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.313
_refine_ls_extinction_coef       0.0018(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   0.695
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         6255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.695
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0350
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.023P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0602
_refine_ls_wR_factor_ref         0.0663
_reflns_number_gt                2931
_reflns_number_total             5013
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            de1212.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Gaussian'
changed to 'gaussian' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2013411