[Ni(MeCN)(H~2~O)~2~(NO~3~)~2~]·(15-crown-5)·MeCN: detailed study of a four-phase sequence that includes an intermediate modulated phase
Siegler, Maxime A.; Parkin, Sean; Brock, Carolyn Pratt; Acta Crystallographica Section B 68 (2012) 389–400; doi:10.1107/S0108768112018319

data_2105172
_publ_section_title
;
 [Ni(MeCN)(H~2~O)~2~(NO~3~)~2~]&#x00B7;(15-crown-5)&#x00B7;MeCN: detailed
 study of a four-phase sequence that includes an intermediate modulated
 phase
;
_journal_coeditor_code           HW5021
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              389
_journal_page_last               400
_journal_paper_doi               10.1107/S0108768112018319
_journal_volume                  68
_journal_year                    2012
_chemical_formula_moiety         'C10 H20 O5, C2 H7 N3 Ni O8, C2 H3 N'
_chemical_formula_sum            'C14 H30 N4 Ni O13'
_chemical_formula_weight         521.13
_chemical_name_systematic
;
acetonitrilediaqual-\k^1^O-nitrato-\k^2^O-nitratonickel(II) (15-crown-5)
acetonitrile solvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb (1/2*x,y,-1/2*x+z)'
_symmetry_space_group_name_H-M   'B 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 and C P Brock'
_cell_angle_alpha                90.
_cell_angle_beta                 122.0260(10)
_cell_angle_gamma                90.
_cell_formula_units_Z            20
_cell_length_a                   27.4626(4)
_cell_length_b                   12.1845(2)
_cell_length_c                   40.2287(6)
_cell_measurement_reflns_used    13682
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     11412.5(3)
_computing_cell_refinement       'DENZO-SMN (Nonius, 1999)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO-SMN (Nonius, 1999)'
_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      90.0(2)
_diffrn_detector_area_resol_mean 18
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.085
_diffrn_reflns_av_sigmaI/netI    0.0860
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -52
_diffrn_reflns_number            25889
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.19
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  0.8519
_exptl_absorpt_correction_T_min  0.7698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 2006)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             5480.1
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.703
_refine_diff_density_min         -0.512
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     962
_refine_ls_number_reflns         25889
_refine_ls_number_restraints     1383
_refine_ls_restrained_S_all      1.110
_refine_ls_R_factor_all          0.1506
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1462
_reflns_number_gt                12328
_reflns_number_total             25889
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            hw5021.cif
_cod_data_source_block           090K_II
_cod_original_sg_symbol_Hall     'B 2yb'
_cod_original_sg_symbol_H-M      'B 21'
_cod_database_code               2105172
_cod_database_fobs_code          2105172