On the sequence of three related phases of [Ni(H~2~O)~2~(15-crown-5)](HSO~4~)~2~ in the temperature range 110–295K
Siegler, Maxime A.; Stavitski, Eli; Acta Crystallographica Section B 66 (2010) 430–440; doi:10.1107/S0108768110020410

data_2104809
_publ_section_title
;
 On the sequence of three related phases of
 [Ni(H~2~O)~2~(15-crown-5)](HSO~4~)~2~ in the temperature range
 110--295K
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              430
_journal_page_last               440
_journal_paper_doi               10.1107/S0108768110020410
_journal_volume                  66
_journal_year                    2010
_chemical_formula_moiety         'C10 H24 Ni O7, 2(H O4 S)'
_chemical_formula_sum            'C10 H26 Ni O15 S2'
_chemical_formula_weight         509.14
_chemical_name_systematic
;
 diaqua(15-crown-5)nickel(II) hydrogen sulfate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.7219(5)
_cell_length_b                   7.5069(3)
_cell_length_c                   14.7170(4)
_cell_measurement_reflns_used    7007
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      1.80
_cell_volume                     1957.90(11)
_computing_cell_refinement       'PEAKREF (Schreurs, 2005)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg et al., 2003)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            15576
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    1.277
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tabular
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.259
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.004(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         4460
_refine_ls_number_restraints     668
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0261
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0260P)^2^+0.7333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                3394
_reflns_number_total             4460
_reflns_threshold_expression     I>2s\s(I)
_cod_data_source_file            zb5013.cif
_cod_data_source_block           II
_cod_database_code               2104809
_cod_database_fobs_code          2104809