Redetermination of <i>catena</i>-poly[[sodium(I)-tri-μ-dimethylformamide-κ^6^<i>O</i>:<i>O</i>] iodide] at 140 K
Chessa, Simona; Wright, Joseph A.; Acta Crystallographica Section E 63 (2007) m787–m789; doi:10.1107/S1600536807007052

data_2212460
_publ_section_title
;Redetermination of
 <i>catena</i>-poly[[sodium(I)-tri-\m-dimethylformamide-\k^6^<i>O</i>:<i>O</i>]
 iodide] at 140 K
;
_journal_coeditor_code           BI2152
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m787
_journal_page_last               m789
_journal_paper_doi               10.1107/S1600536807007052
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Na (C3 H7 N O)3] I'
_chemical_formula_moiety         'C9 H21 N3 Na O3 +, I -'
_chemical_formula_sum            'C9 H21 I N3 Na O3'
_chemical_formula_weight         369.18
_chemical_name_systematic
;
catena-poly[[sodium(I)-tri-\m-dimethylformamide-\k^6^O:O] iodide]
;
_space_group_IT_number           190
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P -6c -2c'
_symmetry_space_group_name_H-M   'P -6 2 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            2
_cell_length_a                   11.8038(14)
_cell_length_b                   11.8038(14)
_cell_length_c                   6.3881(7)
_cell_measurement_reflns_used    4526
_cell_measurement_temperature    140(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      3.76
_cell_volume                     770.81(15)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2006)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis RED'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material
;
SHELXL97, PLATON (Spek, 2003), WinGX (Farrugia, 1999) and
enCIFer (Allen
<i>et al.</i>, 2004)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      140(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur3 CCD'
_diffrn_measurement_method       'Thin-slice \f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0537
_diffrn_reflns_av_sigmaI/netI    0.0248
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            10001
_diffrn_reflns_theta_full        27.60
_diffrn_reflns_theta_max         27.60
_diffrn_reflns_theta_min         3.76
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.107
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.621
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSPACK; Oxford Diffraction, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.350
_refine_ls_abs_structure_details 'Flack (1983), 281 Friedel pairs'
_refine_ls_abs_structure_Flack   0.00(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         657
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0205
_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^)+(0.0162P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0317
_refine_ls_wR_factor_ref         0.0324
_reflns_number_gt                607
_reflns_number_total             657
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bi2152.cif
_cod_data_source_block           I
_cod_database_code               2212460
_cod_database_fobs_code          2212460