({-})-<i>N</i>,<i>N</i>'-Bis[(1<i>S</i>,2<i>R</i>,5<i>S</i>)-6,6-dimethyl-bicyclo[3.1.1]heptan-2-ylmethyl]pyridine-2,6-dicarboxamide monohydrate
Bernès, Sylvain; Pérez-Flores, Francisco Javier; Gutiérrez, René; Acta Crystallographica Section E 64 (2008) o1078–o1079; doi:10.1107/S1600536808013652

data_2218505
_publ_section_title
;({-})-<i>N</i>,<i>N</i>'-Bis[(1<i>S</i>,2<i>R</i>,5<i>S</i>)-6,6-dimethyl-bicyclo[3.1.1]heptan-2-ylmethyl]pyridine-2,6-dicarboxamide
 monohydrate
;
_journal_coeditor_code           RK2088
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1078
_journal_page_last               o1079
_journal_paper_doi               10.1107/S1600536808013652
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C27 H39 N3 O2, H2 O'
_chemical_formula_moiety         'C27 H39 N3 O2, H2 O'
_chemical_formula_sum            'C27 H41 N3 O3'
_chemical_formula_weight         455.63
_chemical_melting_point_gt       398
_chemical_melting_point_lt       401
_chemical_name_systematic
;
(-)-<i>N</i>,<i>N</i>'-Bis[(1<i>S</i>,2<i>R</i>,5<i>S</i>)-6,6-dimethyl-
bicyclo[3.1.1]heptan-2-ylmethyl]pyridine-2,6-dicarboxamide monohydrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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           SHELX
_cell_angle_alpha                90.00
_cell_angle_beta                 91.173(15)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.8476(11)
_cell_length_b                   12.1101(14)
_cell_length_c                   16.012(2)
_cell_measurement_pressure       101(2)
_cell_measurement_reflns_used    60
_cell_measurement_temperature    298.0(10)
_cell_measurement_theta_max      12.49
_cell_measurement_theta_min      4.64
_cell_volume                     1327.5(3)
_computing_cell_refinement       'XSCANS (Siemens, 1996)'
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'XSCANS (Siemens, 1996)'
_computing_molecular_graphics
;
<i>ORTEP-3</i> (Farrugia, 1997) and <i>POV-Ray</i> (Cason, 2004)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.0(10)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_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  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0409
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6391
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.11
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.074
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_density_method    'Not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.135
_refine_diff_density_min         -0.127
_refine_ls_extinction_coef       0.037(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     319
_refine_ls_number_reflns         3180
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0521
_refine_ls_R_factor_gt           0.0396
_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^)+(0.0551P)^2^+0.0694P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1066
_reflns_number_gt                2580
_reflns_number_total             3180
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rk2088.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_matrix_type' value 'Full' changed to 'full' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_weighting_scheme' value 'Calc' changed to 'calc'
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:

'_refine_ls_matrix_type' value 'Full' changed to 'full' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_refine_ls_weighting_scheme' value 'Calc' changed to
'calc' 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_original_sg_symbol_H-M      'P 21'
_cod_database_code               2218505
_cod_database_fobs_code          2218505