#------------------------------------------------------------------------------
#$Date: 2016-02-20 02:53:41 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176768 $
#$URL: svn://www.crystallography.net/cod/cif/2/10/50/2105018.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_2105018
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                 101.200(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.3500(10)
_cell_length_b                   12.5540(10)
_cell_length_c                   8.0930(10)
_cell_measurement_reflns_used    2953
_cell_measurement_temperature    285(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     1230.9(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      285(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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0514
_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            5027
_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    0.872
_exptl_absorpt_correction_T_max  0.9179
_exptl_absorpt_correction_T_min  0.7800
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 2006)'
_exptl_crystal_colour            'pale green'
_exptl_crystal_density_diffrn    1.476
_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         0.912
_refine_diff_density_min         -0.454
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2661
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0681
_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/[σ²(Fo²)+(0.1360P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2219
_reflns_number_gt                1694
_reflns_number_total             2661
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            hw5018.cif
_cod_data_source_block           285K_II
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2105018
_cod_database_fobs_code          2105018
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 0.0709(5) 0.2500 0.7328(6) 0.0973(17) Uani d SU 1 2 . .
C C1 0.0359(6) 0.3435(6) 0.6425(8) 0.116(2) Uani d U 1 1 . .
H H1A -0.0418 0.3557 0.6417 0.140 Uiso calc R 1 1 . .
H H1B 0.0454 0.3362 0.5269 0.140 Uiso calc R 1 1 . .
C C2 0.1022(6) 0.4349(5) 0.7237(8) 0.107(2) Uani d U 1 1 . .
H H2A 0.0744 0.5010 0.6693 0.129 Uiso calc R 1 1 . .
H H2B 0.0973 0.4392 0.8417 0.129 Uiso calc R 1 1 . .
O O2 0.2135(5) 0.4187(4) 0.7078(6) 0.1266(16) Uani d U 1 1 . .
C C3 0.2835(7) 0.4879(7) 0.7903(9) 0.140(2) Uani d U 1 1 . .
H H3A 0.2712 0.4956 0.9045 0.168 Uiso calc R 1 1 . .
H H3B 0.2730 0.5568 0.7354 0.168 Uiso calc R 1 1 . .
C C4 0.3990(6) 0.4486(5) 0.7932(8) 0.124(2) Uani d DU 1 1 . .
H H4A 0.4086 0.4330 0.6796 0.148 Uiso calc R 1 1 A 1
H H4B 0.4520 0.5029 0.8401 0.148 Uiso calc R 1 1 A 1
O O3 0.416(2) 0.3551(17) 0.893(3) 0.143(4) Uani d PDU 0.50 1 . 1
C C5 0.5171(9) 0.2978(11) 0.918(2) 0.154(6) Uani d PDU 0.50 1 . 1
H H5A 0.5564 0.3206 0.8320 0.184 Uiso calc PR 0.50 1 . 1
H H5B 0.5605 0.3206 1.0256 0.184 Uiso calc PR 0.50 1 . 1
O O3' 0.432(2) 0.3657(16) 0.911(3) 0.143(4) Uani d PDU 0.50 1 . 2
C C6 0.4823(17) 0.2972(16) 0.8091(18) 0.261(16) Uani d PDU 0.50 1 . 2
H H6A 0.4517 0.3177 0.6939 0.313 Uiso calc PR 0.50 1 . 2
H H6B 0.5595 0.3177 0.8290 0.313 Uiso calc PR 0.50 1 . 2
Ni Ni 0.25299(5) 0.2500 0.26314(7) 0.0460(4) Uani d S 1 2 . .
O O6 0.2750(4) 0.2500 0.5199(5) 0.0611(11) Uani d SD 1 2 . .
H H6 0.252(3) 0.202(3) 0.576(5) 0.092 Uiso d D 1 1 . .
O O7 0.2362(4) 0.2500 0.0093(5) 0.121(3) Uani d SD 1 2 . .
H H7 0.194(5) 0.2500 -0.079(6) 0.181 Uiso d SD 1 2 . .
H H7' 0.299(3) 0.2500 -0.010(11) 0.181 Uiso d SD 1 2 . .
O O8 0.1345(3) 0.3650(3) 0.2518(4) 0.0695(9) Uani d D 1 1 . .
H H8C 0.081(3) 0.356(4) 0.175(5) 0.104 Uiso d D 1 1 . .
H H8D 0.151(4) 0.4293(19) 0.254(7) 0.104 Uiso d D 1 1 . .
O O9 0.3723(3) 0.1355(3) 0.2771(5) 0.0874(11) Uani d D 1 1 . .
H H9C 0.434(3) 0.146(4) 0.332(7) 0.131 Uiso d D 1 1 . .
H H9D 0.353(5) 0.074(2) 0.277(9) 0.131 Uiso d D 1 1 . .
N N1 0.6304(5) 0.2500 0.4726(8) 0.089(2) Uani d S 1 2 . .
O O12 0.5822(4) 0.3347(4) 0.4490(7) 0.1202(18) Uani d . 1 1 . .
O O13 0.7304(5) 0.2500 0.5317(11) 0.145(3) Uani d S 1 2 . .
N N2 -0.1154(5) 0.2500 0.0293(9) 0.089(2) Uani d S 1 2 . .
O O15 -0.0686(3) 0.3349(3) 0.0627(7) 0.1201(18) Uani d . 1 1 . .
O O16 -0.2104(5) 0.2500 -0.0549(11) 0.146(3) Uani d S 1 2 . .
O O18 0.2380(4) 0.5583(4) 0.2507(6) 0.1193(19) Uani d D 1 1 . .
H H18C 0.264(6) 0.577(6) 0.346(4) 0.179 Uiso d D 1 1 . .
H H18D 0.209(6) 0.611(4) 0.199(7) 0.179 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_565 113.2(7) no
O1 C1 C2 . . 109.1(5) no
O1 C1 H1A . . 109.9 no
C2 C1 H1A . . 109.9 no
O1 C1 H1B . . 109.9 no
C2 C1 H1B . . 109.9 no
H1A C1 H1B . . 108.3 no
O2 C2 C1 . . 108.0(5) no
O2 C2 H2A . . 110.1 no
C1 C2 H2A . . 110.1 no
O2 C2 H2B . . 110.1 no
C1 C2 H2B . . 110.1 no
H2A C2 H2B . . 108.4 no
C3 O2 C2 . . 114.4(6) no
O2 C3 C4 . . 108.7(7) no
O2 C3 H3A . . 110.0 no
C4 C3 H3A . . 110.0 no
O2 C3 H3B . . 110.0 no
C4 C3 H3B . . 110.0 no
H3A C3 H3B . . 108.3 no
O3 C4 O3' . . 10(3) no
O3 C4 C3 . . 108.5(10) no
O3' C4 C3 . . 113.7(10) no
O3 C4 H4A . . 110.0 no
O3' C4 H4A . . 114.6 no
C3 C4 H4A . . 110.0 no
O3 C4 H4B . . 110.0 no
O3' C4 H4B . . 99.6 no
C3 C4 H4B . . 110.0 no
H4A C4 H4B . . 108.4 no
C5 O3 C4 . . 122.2(18) no
C5 C5 O3 4_565 . 120.5(12) no
C5 C5 H5A 4_565 . 107.2 no
O3 C5 H5A . . 107.2 no
C5 C5 H5B 4_565 . 107.2 no
O3 C5 H5B . . 107.2 no
H5A C5 H5B . . 106.8 no
C6 O3' C4 . . 98.9(13) no
C6 C6 O3' 4_565 . 127.4(10) no
C6 C6 H6A 4_565 . 105.5 no
O3' C6 H6A . . 105.5 no
C6 C6 H6B 4_565 . 105.5 no
O3' C6 H6B . . 105.5 no
H6A C6 H6B . . 106.0 no
O7 Ni O8 . . 91.32(14) no
O7 Ni O8 . 4_565 91.32(14) no
O8 Ni O8 . 4_565 89.8(2) no
O7 Ni O9 . . 89.25(16) no
O8 Ni O9 . . 179.36(13) no
O8 Ni O9 4_565 . 90.45(19) no
O7 Ni O9 . 4_565 89.25(16) no
O8 Ni O9 . 4_565 90.45(19) no
O8 Ni O9 4_565 4_565 179.36(13) no
O9 Ni O9 . 4_565 89.3(2) no
O7 Ni O6 . . 178.29(16) no
O8 Ni O6 . . 89.89(13) no
O8 Ni O6 4_565 . 89.89(13) no
O9 Ni O6 . . 89.53(15) no
O9 Ni O6 4_565 . 89.53(15) no
Ni O6 H6 . . 124(3) no
Ni O7 H7 . . 146(6) no
Ni O7 H7' . . 107(6) no
H7 O7 H7' . . 108(4) no
Ni O8 H8C . . 114(4) no
Ni O8 H8D . . 121(4) no
H8C O8 H8D . . 108(3) no
Ni O9 H9C . . 120(4) no
Ni O9 H9D . . 118(5) no
H9C O9 H9D . . 113(4) no
O12 N1 O12 4_565 . 122.1(7) no
O12 N1 O13 4_565 . 118.9(3) no
O12 N1 O13 . . 118.9(3) no
O15 N2 O15 4_565 . 122.2(7) no
O15 N2 O16 4_565 . 118.7(3) no
O15 N2 O16 . . 118.7(3) no
H18C O18 H18D . . 107(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 . 1.406(6) no
O1 C1 4_565 1.406(6) no
C1 C2 . 1.487(9) no
C1 H1A . 0.9700 no
C1 H1B . 0.9700 no
C2 O2 . 1.420(7) no
C2 H2A . 0.9700 no
C2 H2B . 0.9700 no
O2 C3 . 1.313(8) no
C3 C4 . 1.504(10) no
C3 H3A . 0.9700 no
C3 H3B . 0.9700 no
C4 O3 . 1.419(10) no
C4 O3' . 1.419(9) no
C4 H4A . 0.9700 no
C4 H4B . 0.9700 no
O3 C5 . 1.417(10) no
C5 C5 4_565 1.20(3) no
C5 H5A . 0.9700 no
C5 H5B . 0.9700 no
O3' C6 . 1.416(10) no
C6 C6 4_565 1.18(4) no
C6 H6A . 0.9700 no
C6 H6B . 0.9700 no
Ni O7 . 2.024(4) no
Ni O8 . 2.045(3) no
Ni O8 4_565 2.045(3) no
Ni O9 . 2.046(3) no
Ni O9 4_565 2.046(3) no
Ni O6 . 2.043(4) no
O6 H6 . 0.840(19) no
O7 H7 . 0.80(2) no
O7 H7' . 0.82(2) no
O8 H8C . 0.824(19) no
O8 H8D . 0.831(19) no
O9 H9C . 0.812(19) no
O9 H9D . 0.803(19) no
N1 O12 4_565 1.216(5) no
N1 O12 . 1.216(5) no
N1 O13 . 1.235(8) no
N2 O15 4_565 1.217(5) no
N2 O15 . 1.217(5) no
N2 O16 . 1.237(8) no
O18 H18C . 0.81(2) no
O18 H18D . 0.83(2) 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 0.840(19) 1.96(2) 2.797(5) 173(4)
O7 H7 O1 1_554 0.80(2) 1.93(2) 2.720(7) 170(9)
O7 H7' O3 1_554 0.82(2) 2.21(3) 2.90(2) 141(2)
O8 H8C O15 . 0.824(19) 1.91(3) 2.700(5) 160(6)
O8 H8D O18 . 0.831(19) 1.95(3) 2.744(6) 160(6)
O9 H9C O12 4_565 0.812(19) 1.91(2) 2.719(5) 176(7)
O9 H9D O18 4_565 0.803(19) 2.17(3) 2.929(7) 157(6)
O18 H18C O12 3_666 0.81(2) 2.52(5) 3.247(7) 150(8)
O18 H18C O13 3_666 0.81(2) 2.38(6) 2.962(7) 129(6)
O18 H18D O15 3_565 0.83(2) 2.56(4) 3.248(7) 142(6)
O18 H18D O16 3_565 0.83(2) 2.10(4) 2.865(7) 153(8)
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 . -163.6(4) no
O1 C1 C2 O2 . . 65.0(7) no
C1 C2 O2 C3 . . -172.9(7) no
C2 O2 C3 C4 . . 168.2(5) no
O2 C3 C4 O3 . . -67.3(15) no
O2 C3 C4 O3' . . -77.0(15) no
O3' C4 O3 C5 . . -60(7) no
C3 C4 O3 C5 . . 178.9(19) no
C4 O3 C5 C5 . 4_565 -139.8(19) no
O3 C4 O3' C6 . . 73(7) no
C3 C4 O3' C6 . . 135.7(14) no
C4 O3' C6 C6 . 4_565 -144.6(9) no
