#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/50/2105015.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2105015
loop_
_publ_author_name
'Siegler, Maxime A.'
'Hao, Xiang'
'Parkin, Sean'
'Brock, Carolyn Pratt'
_publ_section_title
;
 [Ni(H₂O)₆](NO₃)₂·(15-crown-5)·2H₂O: three phase
 transitions and an intermediate modulated phase stable over a range of
 ca 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           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 100.760(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3190(10)
_cell_length_b                   12.5450(10)
_cell_length_c                   8.0570(10)
_cell_measurement_reflns_used    2938
_cell_measurement_temperature    263(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1223.3(2)
_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      263(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       'ω scans at fixed χ = 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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0476
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5030
_diffrn_reflns_theta_full        26.49
_diffrn_reflns_theta_max         26.49
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        <2
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.9174
_exptl_absorpt_correction_T_min  0.7788
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 2006)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'elongated parallelepiped'
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.483
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2648
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0834
_refine_ls_R_factor_gt           0.0521
_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/[σ²(Fo²)+(0.0752P)²+0.4020P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1309
_refine_ls_wR_factor_ref         0.1482
_reflns_number_gt                1832
_reflns_number_total             2648
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hw5018.cif
_cod_data_source_block           263K_IIb
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2105015
_cod_database_fobs_code          2105015
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
O O1 0.0734(3) 0.2500 0.7386(4) 0.0693(10) Uani d SU 1 2 . .
C C1 0.0355(3) 0.3430(4) 0.6497(5) 0.0876(14) Uani d U 1 1 . .
H H1A -0.0418 0.3546 0.6536 0.105 Uiso calc R 1 1 . .
H H1B 0.0429 0.3363 0.5324 0.105 Uiso calc R 1 1 . .
C C2 0.1031(4) 0.4341(4) 0.7302(6) 0.0923(14) Uani d U 1 1 . .
H H2A 0.0754 0.5005 0.6769 0.111 Uiso calc R 1 1 . .
H H2B 0.0995 0.4380 0.8493 0.111 Uiso calc R 1 1 . .
O O2 0.2141(3) 0.4168(2) 0.7095(4) 0.0844(9) Uani d U 1 1 . .
C C3 0.2885(5) 0.4904(4) 0.7958(6) 0.1070(16) Uani d U 1 1 . .
H H3A 0.2756 0.4996 0.9101 0.128 Uiso calc R 1 1 . .
H H3B 0.2792 0.5589 0.7390 0.128 Uiso calc R 1 1 . .
C C4 0.4028(4) 0.4488(4) 0.7991(6) 0.1047(16) Uani d DU 1 1 . .
H H4A 0.4079 0.4239 0.6868 0.126 Uiso calc R 1 1 A 1
H H4B 0.4548 0.5071 0.8267 0.126 Uiso calc R 1 1 A 1
O O3 0.435(3) 0.364(2) 0.916(4) 0.102(5) Uani d PDU 0.50 1 . 1
C C5 0.5233(6) 0.2878(7) 0.9472(12) 0.098(3) Uani d PDU 0.50 1 . 1
H H5A 0.5702 0.3069 0.8677 0.118 Uiso calc PR 0.50 1 . 1
H H5B 0.5648 0.3069 1.0577 0.118 Uiso calc PR 0.50 1 . 1
O O3' 0.414(3) 0.357(2) 0.903(4) 0.102(5) Uani d PDU 0.50 1 . 2
C C6 0.4991(6) 0.3085(8) 0.8296(10) 0.092(3) Uani d PDU 0.50 1 . 2
H H6A 0.5702 0.3331 0.8905 0.110 Uiso calc PR 0.50 1 . 2
H H6B 0.4916 0.3331 0.7139 0.110 Uiso calc PR 0.50 1 . 2
Ni Ni 0.25465(4) 0.2500 0.27075(6) 0.0417(2) Uani d S 1 2 . .
O O6 0.2789(3) 0.2500 0.5275(3) 0.0442(7) Uani d SD 1 2 . .
H H6 0.254(3) 0.202(2) 0.579(4) 0.066 Uiso d D 1 1 . .
O O7 0.2386(3) 0.2500 0.0161(4) 0.125(2) Uani d SD 1 2 . .
H H7 0.186(4) 0.2500 -0.060(7) 0.187 Uiso d SD 1 2 . .
H H7' 0.293(4) 0.2500 -0.029(9) 0.187 Uiso d SD 1 2 . .
O O8 0.13675(19) 0.3649(2) 0.2615(3) 0.0590(6) Uani d D 1 1 . .
H H8C 0.081(2) 0.355(3) 0.187(4) 0.089 Uiso d D 1 1 . .
H H8D 0.157(3) 0.4264(19) 0.251(5) 0.089 Uiso d D 1 1 . .
O O9 0.3738(2) 0.1359(3) 0.2823(4) 0.0825(9) Uani d D 1 1 . .
H H9C 0.435(2) 0.154(4) 0.331(6) 0.124 Uiso d D 1 1 . .
H H9D 0.359(4) 0.076(2) 0.304(7) 0.124 Uiso d D 1 1 . .
N N1 0.6346(4) 0.2500 0.4723(6) 0.0814(17) Uani d S 1 2 . .
O O12 0.5852(3) 0.3361(3) 0.4543(5) 0.1041(12) Uani d . 1 1 . .
O O13 0.7353(3) 0.2500 0.5208(8) 0.134(2) Uani d S 1 2 . .
N N2 -0.1108(4) 0.2500 0.0231(7) 0.0772(14) Uani d S 1 2 . .
O O15 -0.0643(2) 0.3363(3) 0.0604(4) 0.0966(11) Uani d . 1 1 . .
O O16 -0.2036(4) 0.2500 -0.0678(8) 0.120(2) Uani d S 1 2 . .
O O18 0.2357(3) 0.5582(3) 0.2541(6) 0.1041(12) Uani d D 1 1 . .
H H18C 0.249(5) 0.585(4) 0.346(3) 0.156 Uiso d D 1 1 . .
H H18D 0.201(5) 0.600(4) 0.187(5) 0.156 Uiso d D 1 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 O1 C1 4_565 . 112.5(5) no
O1 C1 C2 . . 108.1(3) no
O1 C1 H1A . . 110.1 no
C2 C1 H1A . . 110.1 no
O1 C1 H1B . . 110.1 no
C2 C1 H1B . . 110.1 no
H1A C1 H1B . . 108.4 no
O2 C2 C1 . . 107.6(3) no
O2 C2 H2A . . 110.2 no
C1 C2 H2A . . 110.2 no
O2 C2 H2B . . 110.2 no
C1 C2 H2B . . 110.2 no
H2A C2 H2B . . 108.5 no
C3 O2 C2 . . 113.4(4) no
O2 C3 C4 . . 107.9(4) no
O2 C3 H3A . . 110.1 no
C4 C3 H3A . . 110.1 no
O2 C3 H3B . . 110.1 no
C4 C3 H3B . . 110.1 no
H3A C3 H3B . . 108.4 no
O3' C4 O3 . . 11(4) no
O3' C4 C3 . . 106.5(9) no
O3 C4 C3 . . 114.4(8) no
O3' C4 H4A . . 105.7 no
O3 C4 H4A . . 108.7 no
C3 C4 H4A . . 108.7 no
O3' C4 H4B . . 119.3 no
O3 C4 H4B . . 108.7 no
C3 C4 H4B . . 108.7 no
H4A C4 H4B . . 107.6 no
C4 O3 C5 . . 135.9(11) no
C5 C5 O3 4_565 . 131.8(18) no
C5 C5 H5A 4_565 . 104.3 no
O3 C5 H5A . . 104.3 no
C5 C5 H5B 4_565 . 104.3 no
O3 C5 H5B . . 104.3 no
H5A C5 H5B . . 105.6 no
C4 O3' C6 . . 95.7(8) no
O3' C6 C6 . 4_565 115.0(13) no
O3' C6 H6A . . 108.5 no
C6 C6 H6A 4_565 . 108.5 no
O3' C6 H6B . . 108.5 no
C6 C6 H6B 4_565 . 108.5 no
H6A C6 H6B . . 107.5 no
O7 Ni O6 . . 177.23(13) no
O7 Ni O9 . . 88.84(12) no
O6 Ni O9 . . 89.18(11) no
O7 Ni O9 . 4_565 88.84(12) no
O6 Ni O9 . 4_565 89.18(11) no
O9 Ni O9 . 4_565 89.14(19) no
O7 Ni O8 . . 91.63(10) no
O6 Ni O8 . . 90.32(9) no
O9 Ni O8 . . 179.34(10) no
O9 Ni O8 4_565 . 90.41(13) no
O7 Ni O8 . 4_565 91.63(10) no
O6 Ni O8 . 4_565 90.32(9) no
O9 Ni O8 . 4_565 90.41(13) no
O9 Ni O8 4_565 4_565 179.34(10) no
O8 Ni O8 . 4_565 90.03(14) no
Ni O6 H6 . . 121(2) no
Ni O7 H7 . . 133(6) no
Ni O7 H7' . . 121(6) no
H7 O7 H7' . . 106(4) no
Ni O8 H8C . . 114(3) no
Ni O8 H8D . . 116(3) no
H8C O8 H8D . . 107(3) no
Ni O9 H9C . . 115(4) no
Ni O9 H9D . . 118(4) no
H9C O9 H9D . . 113(4) no
O12 N1 O12 4_565 . 122.1(5) no
O12 N1 O13 4_565 . 118.9(3) no
O12 N1 O13 . . 118.9(3) no
O15 N2 O15 4_565 . 122.5(5) no
O15 N2 O16 4_565 . 118.6(2) no
O15 N2 O16 . . 118.6(2) no
H18C O18 H18D . . 109(4) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
O1 C1 4_565 1.402(4) no
O1 C1 . 1.402(4) no
C1 C2 . 1.489(6) no
C1 H1A . 0.9700 no
C1 H1B . 0.9700 no
C2 O2 . 1.424(5) no
C2 H2A . 0.9700 no
C2 H2B . 0.9700 no
O2 C3 . 1.392(5) no
C3 C4 . 1.497(7) no
C3 H3A . 0.9700 no
C3 H3B . 0.9700 no
C4 O3' . 1.420(9) no
C4 O3 . 1.426(9) no
C4 H4A . 0.9700 no
C4 H4B . 0.9700 no
O3 C5 . 1.439(9) no
C5 C5 4_565 0.948(18) no
C5 H5A . 0.9700 no
C5 H5B . 0.9700 no
O3' C6 . 1.428(10) no
C6 C6 4_565 1.468(19) no
C6 H6A . 0.9700 no
C6 H6B . 0.9700 no
Ni O7 . 2.024(3) no
Ni O6 . 2.034(3) no
Ni O9 . 2.040(3) no
Ni O9 4_565 2.040(3) no
Ni O8 . 2.037(2) no
Ni O8 4_565 2.037(2) no
O6 H6 . 0.821(17) no
O7 H7 . 0.80(2) no
O7 H7' . 0.82(2) no
O8 H8C . 0.830(18) no
O8 H8D . 0.820(18) no
O9 H9C . 0.810(18) no
O9 H9D . 0.798(19) no
N1 O12 4_565 1.234(4) no
N1 O12 . 1.234(4) no
N1 O13 . 1.229(6) no
N2 O15 4_565 1.235(3) no
N2 O15 . 1.235(3) no
N2 O16 . 1.238(6) no
O18 H18C . 0.804(19) no
O18 H18D . 0.818(19) no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O6 H6 O2 4_565 0.821(17) 1.941(18) 2.757(3) 173(3)
O7 H7 O1 1_554 0.80(2) 1.93(2) 2.728(5) 173(8)
O7 H7' O3 1_554 0.82(2) 2.36(4) 3.04(3) 141(2)
O8 H8C O15 . 0.830(18) 1.90(2) 2.719(4) 167(4)
O8 H8D O18 . 0.820(18) 1.915(19) 2.721(4) 167(4)
O9 H9C O12 4_565 0.810(18) 1.94(2) 2.735(4) 168(5)
O9 H9D O18 4_565 0.798(19) 2.25(3) 2.955(5) 147(5)
O18 H18C O12 3_666 0.804(19) 2.55(4) 3.195(5) 138(6)
O18 H18C O13 3_666 0.804(19) 2.32(4) 2.994(5) 142(5)
O18 H18D O15 3_565 0.818(19) 2.49(2) 3.260(5) 158(5)
O18 H18D O16 3_565 0.818(19) 2.11(4) 2.824(5) 145(6)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
C1 O1 C1 C2 4_565 . -164.8(3) no
O1 C1 C2 O2 . . 64.1(4) no
C1 C2 O2 C3 . . -173.2(4) no
C2 O2 C3 C4 . . 166.5(4) no
O2 C3 C4 O3' . . -67(2) no
O2 C3 C4 O3 . . -76(2) no
O3' C4 O3 C5 . . 122(16) no
C3 C4 O3 C5 . . 167(4) no
C4 O3 C5 C5 . 4_565 -121(4) no
O3 C4 O3' C6 . . -67(9) no
C3 C4 O3' C6 . . 155.9(18) no
C4 O3' C6 C6 . 4_565 -149.0(16) no
