Hexakis(urea-κ<i>O</i>)zinc(II) dinitrate at 110 and 250K: uniaxial negative thermal expansion
Smeets, Stef; Lutz, Martin; Acta Crystallographica Section C 67 (2011) m50–m55; doi:10.1107/S0108270111000023

data_2017978
_publ_section_title
;
 Hexakis(urea-\k<i>O</i>)zinc(II) dinitrate at 110 and 250K: uniaxial
 negative thermal expansion
;
_journal_coeditor_code           FN3074
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m50
_journal_page_last               m55
_journal_paper_doi               10.1107/S0108270111000023
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Zn (C H4 N2 O1)6] (N O3)2'
_chemical_formula_moiety         'C6 H24 N12 O6 Zn 2+, 2(N O3 -)'
_chemical_formula_sum            'C6 H24 N14 O12 Zn'
_chemical_formula_weight         549.76
_chemical_name_systematic
;
Hexakis(urea-\k<i>O</i>)zinc(II) dinitrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.701(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1082(6)
_cell_length_b                   17.9456(7)
_cell_length_c                   7.46654(16)
_cell_measurement_reflns_used    33077
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      35.03
_cell_measurement_theta_min      1.70
_cell_volume                     2158.17(13)
_computing_cell_refinement       'PEAKREF (Schreurs, 2008)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction
;
EVAL15 (Schreurs <i>et al.</i>, 2010) and SADABS (Sheldrick,
2008<i>a</i>)
;
_computing_molecular_graphics
;
PLATON (Spek, 2009) and Jmol (Jmol, 2010)
;
_computing_publication_material  'manual editing of SHELXL97 cif file'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008<i>b</i>)'
_computing_structure_solution
'coordinates from literature (van de Giesen & Stam, 1972)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            41204
_diffrn_reflns_theta_full        35.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.6680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008<i>a</i>)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.692
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         4747
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0391
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0386P)^2^+0.8626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0747
_reflns_number_gt                4013
_reflns_number_total             4747
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fn3074.cif
_cod_data_source_block           Ib
_cod_original_cell_volume        2158.18(12)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2017978
_cod_database_fobs_code          2017978