Three modulation patterns in four related [<i>M</i>(H~2~O)~2~(15-crown-5)](NO~3~)~2~ structures
Hao, Xiang; Parkin, Sean; Brock, Carolyn Pratt; Acta Crystallographica Section B 61 (2005) 675–688; doi:10.1107/S0108768105026662

data_2100297
_publ_section_title
;
 Three modulation patterns in four related
 [<i>M</i>(H~2~O)~2~(15-crown-5)](NO~3~)~2~ structures
;
_journal_coeditor_code           BM5026
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              675
_journal_page_last               688
_journal_paper_doi               10.1107/S0108768105026662
_journal_volume                  61
_journal_year                    2005
_chemical_formula_moiety         '(C10 H24 O7 Mg 2+), 2(N O3 1-)'
_chemical_formula_sum            'C10 H24 Mg N2 O13'
_chemical_formula_weight         404.62
_chemical_name_systematic
;
 diaqua(15-crown-5)magnesium(II) nitrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.46(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   14.497(3)
_cell_length_b                   14.181(3)
_cell_length_c                   25.700(5)
_cell_measurement_reflns_used    23626
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     5249.9(19)
_computing_cell_refinement       'SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in Siemens SHELXTL (Sheldrick, 1994)'
_computing_publication_material
;
SHELX97-2 (Sheldrick, 1997) and local procedures
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\w scans at fixed \c = 55\%'
_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  0.1027
_diffrn_reflns_av_sigmaI/netI    0.0843
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            46462
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_T_max  0.9829
_exptl_absorpt_correction_T_min  0.9499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.236
_refine_diff_density_min         -0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     740
_refine_ls_number_reflns         12054
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.1341
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0414P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.1057
_reflns_number_gt                5815
_reflns_number_total             12054
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            bm5026.cif
_cod_data_source_block           k02119
_cod_original_cell_volume        5249.9(18)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2100297
_cod_database_fobs_code          2100297