#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:29:43 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229110 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/05/7230565.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7230565
loop_
_publ_author_name
'Daszkiewicz, Marek'
'Puszyńska-Tuszkanow, Mariola'
'Staszak, Zbigniew'
'Chojnacka, Ida'
'Fałtynowicz, Hanna'
'Cieślak-Golonka, Maria'
_publ_section_title
;
 Single crystal-to-single crystal transformations induced by
 ammonia--water equilibrium changes
;
_journal_issue                   21
_journal_name_full               CrystEngComm
_journal_page_first              2907
_journal_paper_doi               10.1039/C8CE00401C
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         'C20 H28 N6 Ni O6, 1.23(N H3)'
_chemical_formula_sum            'C20 H31.66 N7.23 Ni O6'
_chemical_formula_weight         528.11
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-03-13 deposited with the CCDC.
2018-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                95.898(12)
_cell_angle_beta                 91.502(13)
_cell_angle_gamma                99.545(14)
_cell_formula_units_Z            1
_cell_length_a                   6.7306(12)
_cell_length_b                   8.9921(13)
_cell_length_c                   10.4338(15)
_cell_measurement_reflns_used    2107
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.73
_cell_measurement_theta_min      3.07
_cell_volume                     618.84(17)
_computing_cell_refinement       'CrysAlis 1.171.32.6'
_computing_data_collection       'CrysAlis 1.171.32.6'
_computing_data_reduction        'CrysAlis 1.171.32.6'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2, 33.133pixel/mm'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       ω-scan
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7749
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         3.072
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.833
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.824
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'CrysAlis 1.171.32.6'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       prism
_exptl_crystal_F_000             278
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2611
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0718P)²+0.3075P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1394
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2107
_reflns_number_total             2611
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8ce00401c2.cif
_cod_data_source_block           Ni_1
_cod_depositor_comments
'Adding full bibliography for 7230563--7230565.cif.'
_cod_database_code               7230565
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ni1 Ni 0.0000 0.0000 0.5000 0.0434(2) Uani 1 2 d S . P
N1 N -0.1839(4) -0.1072(3) 0.8841(2) 0.0493(7) Uani 1 1 d . . .
H1 H -0.1624 -0.0965 0.9664 0.059 Uiso 1 1 calc R U .
C2 C -0.0676(5) -0.0284(3) 0.8018(2) 0.0385(6) Uani 1 1 d . . .
O2 O 0.0816(3) 0.0686(2) 0.83610(19) 0.0482(5) Uani 1 1 d . . .
N3 N -0.1400(4) -0.0709(3) 0.6748(2) 0.0404(6) Uani 1 1 d . . .
C4 C -0.3047(5) -0.1760(3) 0.6773(3) 0.0431(7) Uani 1 1 d . . .
O4 O -0.4143(4) -0.2384(3) 0.5843(2) 0.0621(7) Uani 1 1 d . . .
C5 C -0.3489(5) -0.2117(3) 0.8166(3) 0.0440(7) Uani 1 1 d . . .
C11 C -0.5513(6) -0.1677(4) 0.8528(4) 0.0596(9) Uani 1 1 d . . .
H11A H -0.5849 -0.1983 0.9361 0.089 Uiso 1 1 calc R U .
H11B H -0.6540 -0.2173 0.7898 0.089 Uiso 1 1 calc R U .
H11C H -0.5424 -0.0597 0.8552 0.089 Uiso 1 1 calc R U .
C21 C -0.3354(5) -0.3768(3) 0.8281(3) 0.0430(7) Uani 1 1 d . . .
C22 C -0.5040(6) -0.4876(4) 0.8165(4) 0.0681(10) Uani 1 1 d . . .
H22 H -0.6306 -0.4610 0.8053 0.082 Uiso 1 1 calc R U .
C23 C -0.4872(8) -0.6389(5) 0.8212(5) 0.0842(14) Uani 1 1 d . . .
H23 H -0.6030 -0.7123 0.8134 0.101 Uiso 1 1 calc R U .
C24 C -0.3041(8) -0.6812(4) 0.8369(4) 0.0710(12) Uani 1 1 d . . .
H24 H -0.2935 -0.7829 0.8381 0.085 Uiso 1 1 calc R U .
C25 C -0.1387(7) -0.5733(5) 0.8506(4) 0.0744(11) Uani 1 1 d . . .
H25 H -0.0130 -0.6008 0.8633 0.089 Uiso 1 1 calc R U .
C26 C -0.1520(6) -0.4219(4) 0.8461(4) 0.0638(9) Uani 1 1 d . . .
H26 H -0.0351 -0.3496 0.8554 0.077 Uiso 1 1 calc R U .
N1A N -0.0047(8) -0.2290(4) 0.4333(4) 0.1085(18) Uani 1 1 d . . .
H1A1 H 0.1069 -0.2582 0.4620 0.130 Uiso 1 1 calc R U .
H2A1 H -0.0108 -0.2404 0.3475 0.130 Uiso 1 1 calc R U .
H3A1 H -0.1121 -0.2855 0.4622 0.130 Uiso 1 1 calc R U .
O1W O -0.2833(5) -0.0174(5) 0.4084(3) 0.1015(12) Uani 1 1 d . . .
H1W1 H -0.3700 -0.0920 0.4419 0.122 Uiso 1 1 d . U .
H2W1 H -0.2801 -0.0479 0.3230 0.122 Uiso 1 1 d . U .
N2A N 0.2545(10) 0.5454(8) 0.5131(7) 0.088(3) Uani 0.613(14) 1 d . . P
H1N2 H 0.3307 0.6280 0.5438 0.131 Uiso 0.6128 1 d . U P
H2N2 H 0.3157 0.4719 0.5275 0.131 Uiso 0.6128 1 d . U P
H3N2 H 0.2268 0.5442 0.4340 0.131 Uiso 0.6128 1 d . U P
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1W Ni1 O1W 180.0(2) . 2_556
O1W Ni1 N1A 88.1(2) . .
O1W Ni1 N1A 91.9(2) 2_556 .
O1W Ni1 N1A 91.9(2) . 2_556
O1W Ni1 N1A 88.1(2) 2_556 2_556
N1A Ni1 N1A 180.0 . 2_556
O1W Ni1 N3 90.48(11) . .
O1W Ni1 N3 89.52(11) 2_556 .
N1A Ni1 N3 89.07(11) . .
N1A Ni1 N3 90.93(11) 2_556 .
O1W Ni1 N3 89.52(11) . 2_556
O1W Ni1 N3 90.48(11) 2_556 2_556
N1A Ni1 N3 90.93(11) . 2_556
N1A Ni1 N3 89.08(11) 2_556 2_556
N3 Ni1 N3 180.0 . 2_556
C2 N1 C5 111.6(2) . .
C2 N1 H1 124.2 . .
C5 N1 H1 124.2 . .
O2 C2 N1 123.9(3) . .
O2 C2 N3 125.2(2) . .
N1 C2 N3 110.9(3) . .
C4 N3 C2 107.3(2) . .
C4 N3 Ni1 124.88(18) . .
C2 N3 Ni1 127.53(19) . .
O4 C4 N3 126.8(3) . .
O4 C4 C5 121.9(3) . .
N3 C4 C5 111.3(2) . .
N1 C5 C21 113.0(3) . .
N1 C5 C11 110.9(3) . .
C21 C5 C11 114.2(3) . .
N1 C5 C4 98.9(2) . .
C21 C5 C4 109.3(2) . .
C11 C5 C4 109.4(3) . .
C5 C11 H11A 109.5 . .
C5 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C5 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C22 C21 C26 117.3(3) . .
C22 C21 C5 121.6(3) . .
C26 C21 C5 121.0(3) . .
C21 C22 C23 120.7(4) . .
C21 C22 H22 119.7 . .
C23 C22 H22 119.7 . .
C24 C23 C22 121.0(4) . .
C24 C23 H23 119.5 . .
C22 C23 H23 119.5 . .
C25 C24 C23 118.7(4) . .
C25 C24 H24 120.7 . .
C23 C24 H24 120.7 . .
C24 C25 C26 121.2(4) . .
C24 C25 H25 119.4 . .
C26 C25 H25 119.4 . .
C21 C26 C25 121.0(4) . .
C21 C26 H26 119.5 . .
C25 C26 H26 119.5 . .
Ni1 N1A H1A1 109.5 . .
Ni1 N1A H2A1 109.5 . .
H1A1 N1A H2A1 109.5 . .
Ni1 N1A H3A1 109.5 . .
H1A1 N1A H3A1 109.5 . .
H2A1 N1A H3A1 109.5 . .
Ni1 O1W H1W1 108.2 . .
Ni1 O1W H2W1 111.1 . .
H1W1 O1W H2W1 106.1 . .
H1N2 N2A H2N2 107.5 . .
H1N2 N2A H3N2 111.9 . .
H2N2 N2A H3N2 111.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1W 2.085(3) .
Ni1 O1W 2.085(3) 2_556
Ni1 N1A 2.100(3) .
Ni1 N1A 2.100(3) 2_556
Ni1 N3 2.179(2) .
Ni1 N3 2.179(2) 2_556
N1 C2 1.353(3) .
N1 C5 1.445(4) .
N1 H1 0.8600 .
C2 O2 1.235(4) .
C2 N3 1.393(4) .
N3 C4 1.335(4) .
C4 O4 1.230(4) .
C4 C5 1.546(4) .
C5 C21 1.519(4) .
C5 C11 1.526(5) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C21 C22 1.374(5) .
C21 C26 1.376(5) .
C22 C23 1.389(6) .
C22 H22 0.9300 .
C23 C24 1.360(7) .
C23 H23 0.9300 .
C24 C25 1.344(6) .
C24 H24 0.9300 .
C25 C26 1.384(6) .
C25 H25 0.9300 .
C26 H26 0.9300 .
N1A H1A1 0.8900 .
N1A H2A1 0.8900 .
N1A H3A1 0.8900 .
O1W H1W1 0.9173 .
O1W H2W1 0.9070 .
N2A H1N2 0.8564 .
N2A H2N2 0.8585 .
N2A H3N2 0.8394 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1 O2 0.86 2.10 2.953(3) 174.7 2_557
N1A H1A1 N2A 0.89 2.27 3.049(9) 146.5 1_545
N1A H3A1 N2A 0.89 2.42 3.166(8) 142.0 2_556
N1A H3A1 O4 0.89 2.50 3.205(5) 136.4 .
O1W H1W1 O4 0.92 2.08 2.889(4) 146.5 .
O1W H2W1 O2 0.91 2.17 2.951(4) 143.8 2_556
N2A H1N2 O4 0.86 1.93 2.736(6) 155.1 1_665
N2A H2N2 O4 0.86 2.49 3.206(8) 141.1 2_556
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
C5 N1 C2 O2 179.4(3)
C5 N1 C2 N3 -0.2(4)
O2 C2 N3 C4 -178.8(3)
N1 C2 N3 C4 0.8(3)
O2 C2 N3 Ni1 6.9(4)
N1 C2 N3 Ni1 -173.5(2)
C2 N3 C4 O4 177.9(3)
Ni1 N3 C4 O4 -7.6(5)
C2 N3 C4 C5 -1.0(3)
Ni1 N3 C4 C5 173.48(19)
C2 N1 C5 C21 115.1(3)
C2 N1 C5 C11 -115.1(3)
C2 N1 C5 C4 -0.4(3)
O4 C4 C5 N1 -178.1(3)
N3 C4 C5 N1 0.9(3)
O4 C4 C5 C21 63.6(4)
N3 C4 C5 C21 -117.5(3)
O4 C4 C5 C11 -62.2(4)
N3 C4 C5 C11 116.8(3)
N1 C5 C21 C22 154.6(3)
C11 C5 C21 C22 26.5(4)
C4 C5 C21 C22 -96.4(4)
N1 C5 C21 C26 -27.8(4)
C11 C5 C21 C26 -155.8(3)
C4 C5 C21 C26 81.3(4)
C26 C21 C22 C23 -0.9(6)
C5 C21 C22 C23 176.9(4)
C21 C22 C23 C24 -0.2(7)
C22 C23 C24 C25 1.4(7)
C23 C24 C25 C26 -1.4(7)
C22 C21 C26 C25 0.8(6)
C5 C21 C26 C25 -177.0(3)
C24 C25 C26 C21 0.3(6)
