[Ni(H~2~O)~6~](NO~3~)~2~·(15-crown-5)·2H~2~O: three phase transitions and an intermediate modulated phase stable over a range of <i>ca</i> 40K
Siegler, Maxime A.; Hao, Xiang; Parkin, Sean; Brock, Carolyn Pratt; Acta Crystallographica Section B 67 (2011) 486–498; doi:10.1107/S0108768111045897

data_2105001
_publ_section_title
;
 [Ni(H~2~O)~6~](NO~3~)~2~&#x00B7;(15-crown-5)&#x00B7;2H~2~O: three phase
 transitions and an intermediate modulated phase stable over a range of
 <i>ca</i> 40K
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              486
_journal_page_last               498
_journal_paper_doi               10.1107/S0108768111045897
_journal_volume                  67
_journal_year                    2011
_chemical_formula_moiety         'C10 H20 O5, H12 Ni O6 2+, 2(N O3 1-), 2(H2 O)'
_chemical_formula_sum            'C10 H36 N2 Ni O19'
_chemical_formula_weight         547.12
_chemical_name_systematic
'hexaquanickel(II) nitrate (15-crown-5) dihydrate'
_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                 101.54(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.981(2)
_cell_length_b                   12.688(2)
_cell_length_c                   15.999(2)
_cell_measurement_reflns_used    5716
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     2382.9(6)
_computing_cell_refinement       'DENZO-SMN (Nonius, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        'DENZO-SMN (Nonius, 1997)'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELX-97 and local procedures'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(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  0.0330
_diffrn_reflns_av_sigmaI/netI    0.0468
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10682
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  0.8062
_exptl_absorpt_correction_T_min  0.7146
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 2006)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.525
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated parallelepiped'
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.632
_refine_diff_density_min         -0.518
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         5466
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0478P)^2^+0.3043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                3934
_reflns_number_total             5466
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hw5018.cif
_cod_data_source_block           120K_IV
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2105001
_cod_database_fobs_code          2105001