Reaction of [Ni(H2O)6](NO3)2 with gaseous NH3; crystal growth via in-situ solvation
Breternitz, Joachim; Farrugia, Louis J.; Godula-Jopek, Agata; Saremi-Yarahmadi, Sina; Malka, Iwona E.; Hoang, Tuan K.A.; Gregory, Duncan H.; Journal of Crystal Growth 412 (2015) 1–; doi:10.1016/j.jcrysgro.2014.11.021

data_1518683
_publ_section_title
;
 Reaction of [Ni(H2O)6](NO3)2 with gaseous NH3; crystal growth via in-situ
 solvation
;
_journal_name_full               'Journal of Crystal Growth'
_journal_page_first              1
_journal_paper_doi               10.1016/j.jcrysgro.2014.11.021
_journal_volume                  412
_journal_year                    2015
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'H12 Ni O6, 2(N O3)'
_chemical_formula_sum            'H12 N2 Ni O12'
_chemical_formula_weight         290.83
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.2
_audit_creation_date             2013-04-30T11:08:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                106.347(2)
_cell_angle_beta                 98.450(2)
_cell_angle_gamma                101.538(2)
_cell_formula_units_Z            2
_cell_length_a                   5.7531(3)
_cell_length_b                   7.6604(4)
_cell_length_c                   11.4876(6)
_cell_measurement_reflns_used    9604
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      60.88
_cell_measurement_theta_min      2.88
_cell_measurement_wavelength     0.71073
_cell_volume                     464.73(4)
_computing_cell_refinement
'SAINT V8.27B integration software (Bruker, 2012)'
_computing_data_collection       'Bruker APEX2 software (Bruker, 2012)'
_computing_data_reduction        'SORTAV (Blessing, 1987)'
_computing_molecular_graphics    'Diamond 3.1 (Brandenburg, 2005)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'APEX-II CCD'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       '\f or \w oscillation scans'
_diffrn_orient_matrix_UB_11      0.16623
_diffrn_orient_matrix_UB_12      0.085827
_diffrn_orient_matrix_UB_13      0.019345
_diffrn_orient_matrix_UB_21      -0.009341
_diffrn_orient_matrix_UB_22      0.048019
_diffrn_orient_matrix_UB_23      0.089195
_diffrn_orient_matrix_UB_31      0.072769
_diffrn_orient_matrix_UB_32      -0.100573
_diffrn_orient_matrix_UB_33      0.017413
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            32234
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_reduction_process
;
        Scaled and merged with Sortav
        R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
        R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         60.935
_diffrn_reflns_theta_min         1.892
_diffrn_source                   'sealed x-ray tube'
_exptl_absorpt_coefficient_mu    2.155
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.575
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.078
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             300
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.4
_refine_diff_density_max         2.264
_refine_diff_density_min         -1.118
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     185
_refine_ls_number_reflns         13670
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+0.0544P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1015
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                12467
_reflns_number_total             13670
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            hydrates.cif
_cod_data_source_block           100K
_cod_database_code               1518683