Tryptophan moiety ligand based tri/tetranuclear Ni(ii) complexes: syntheses, structure and magnetic properties
Mahish, Manas Kumar; Carrella, Luca M.; Patra, Apu; Saren, Dama; Zangrando, Ennio; Vojtíšek, Pavel; Rentschler, Eva; Manna, Subal Chandra; New Journal of Chemistry 46 (2022) 16899–16906; doi:10.1039/D2NJ02467E

data_7061752
_publ_section_title
;
 Tryptophan moiety ligand based tri/tetranuclear Ni(ii) complexes:
 syntheses, structure and magnetic properties
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              16899
_journal_page_last               16906
_journal_paper_doi               10.1039/D2NJ02467E
_journal_volume                  46
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C76 H72 N8 Ni4 O20, 5(C3 H7 N O), 7(H2 O)'
_chemical_formula_sum            'C91 H121 N13 Ni4 O32'
_chemical_formula_weight         2143.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-04-28 deposited with the CCDC.	2022-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 116.6750(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.8669(6)
_cell_length_b                   22.8072(10)
_cell_length_c                   16.0694(6)
_cell_measurement_reflns_used    4720
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.55
_cell_measurement_theta_min      2.92
_cell_volume                     4868.8(3)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'Ortep3/Windows (Farrugia,1997)'
_computing_publication_material  'Wingx 2018.3 (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD with Bruker APEXII'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            94650
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.543
_diffrn_reflns_theta_min         2.281
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_T_max  0.796
_exptl_absorpt_correction_T_min  0.675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             2252
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.323
_exptl_crystal_size_min          0.208
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 9668 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0141(18)
_refine_ls_extinction_coef       0.0025(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1306
_refine_ls_number_reflns         22399
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+2.1830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0707
_refine_ls_wR_factor_ref         0.0727
_reflns_Friedel_coverage         0.948
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                21194
_reflns_number_total             22399
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj02467e2.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 

 Adding full bibliography for 7061752--7061753.cif.
;
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7061752
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.754
_shelx_estimated_absorpt_t_max   0.843
_shelx_res_checksum              4602