Single crystal-to-single crystal transformations induced by ammonia‒water equilibrium changes
Daszkiewicz, Marek; Puszyńska-Tuszkanow, Mariola; Staszak, Zbigniew; Chojnacka, Ida; Fałtynowicz, Hanna; Cieślak-Golonka, Maria; CrystEngComm 20 (2018) 2907–; doi:10.1039/C8CE00401C

data_7230565
_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       \w-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/[\s^2^(Fo^2^)+(0.0718P)^2^+0.3075P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_res_checksum              32924