Investigating the isolation and interconversion of two diastereoisomers in an octahedral system
Danelli, Panagiota; Tsantis, Sokratis T.; Kitos, Alexandros; Psycharis, Vassilis; Raptopoulou, Catherine P.; Tsipis, Athanassios; Perlepes, Spyros P.; New Journal of Chemistry 43 (2019) 17141–17145; doi:10.1039/C9NJ04876F

data_7058916
_publ_section_title
;
 Investigating the isolation and interconversion of two diastereoisomers
 in an octahedral system
;
_journal_issue                   44
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17141
_journal_page_last               17145
_journal_paper_doi               10.1039/C9NJ04876F
_journal_volume                  43
_journal_year                    2019
_chemical_formula_sum            'C25.2 H22.4 Cl2 N2 Ni O3'
_chemical_formula_weight         530.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-10-14 deposited with the CCDC.    2019-10-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.3620(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5379(2)
_cell_length_b                   9.1919(2)
_cell_length_c                   25.3211(5)
_cell_measurement_reflns_used    15663
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      3.00
_cell_volume                     2441.95(9)
_computing_cell_refinement       'CrystalClear, Rigaku MSC 2005'
_computing_data_collection       'CrystalClear, Rigaku MSC 2005'
_computing_data_reduction        'CrystalClear, Rigaku MSC 2005'
_computing_molecular_graphics    'Diamond ver.3.1'
_computing_publication_material  'publCIF J.Appl.Cryst. 2010, 43, 920-925'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2013/1 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS SPIDER IPDS'
_diffrn_measurement_method       '\q scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21709
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         3.007
_exptl_absorpt_coefficient_mu    1.043
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.740
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrystalClear, Rigaku MSC 2005'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.224
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5319
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+2.0997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1258
_refine_ls_wR_factor_ref         0.1441
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4036
_reflns_number_total             5319
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04876f2.cif
_cod_data_source_block           shelx
_cod_original_formula_sum        'C25.20 H22.40 Cl2 N2 Ni O3'
_cod_database_code               7058916
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              11908