Gradual Transition from NH···Pyridyl Hydrogen Bonding to the NH···O Tape Synthon in Pyridyl Ureas
Byrne, Peter; Turner, David R.; Lloyd, Gareth O.; Clarke, Nigel; Steed, Jonathan W.; Crystal Growth & Design 8 (2008) 3335–; doi:10.1021/cg800247f

data_4503672
_publ_section_title
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 Gradual Transition from NH&#x00B7;&#x00B7;&#x00B7;Pyridyl Hydrogen
 Bonding to the NH&#x00B7;&#x00B7;&#x00B7;O Tape Synthon in Pyridyl Ureas
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_journal_issue                   9
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              3335
_journal_paper_doi               10.1021/cg800247f
_journal_volume                  8
_journal_year                    2008
_chemical_formula_sum            'C26 H28 F6 N6 O2 Si'
_chemical_formula_weight         598.63
_chemical_name_common            m-TUP_SiF6
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                70.07(3)
_cell_angle_beta                 83.74(3)
_cell_angle_gamma                86.46(3)
_cell_formula_units_Z            2
_cell_length_a                   7.3551(15)
_cell_length_b                   13.731(3)
_cell_length_c                   13.869(3)
_cell_measurement_temperature    120(2)
_cell_volume                     1308.5(5)
_computing_cell_refinement       'SMART for WNT/2000 (Bruker, 2003)'
_computing_data_collection       'SMART for WNT/2000 (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'X-Seed (Barbour)'
_computing_publication_material  'Cif2Cif (Barbour)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker SMART 1K CCD'
_diffrn_measurement_method       \w
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9013
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  0.9831
_exptl_absorpt_correction_T_min  0.9748
_exptl_absorpt_correction_type   'Semi-empirical from equivalents'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.050
_refine_ls_extinction_coef       0.010(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         5866
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0423P)^2^+0.5591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                5093
_reflns_number_total             5866
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg800247f_si_010.cif
_cod_data_source_block           SIF6
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4503672