Crystal structure of aqua(μ2-2,2′,2″-((nitrilo)tris(ethane-2,1-diyl(nitrilo)methylylidene))tris (6-ethoxyphenolato))(pentane-2,4-dionato-κ2 O,O′)-dinickel(II), C38H48N4Ni2O9
Ha, Kwang; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 407–409; doi:10.1515/ncrs-2023-0043

data_8107454
_publ_section_title
;
 Crystal structure of
 aqua(\m2-2,2&#x2032;,2&#x2033;-((nitrilo)tris(ethane-2,1-diyl(nitrilo)methylylidene))tris
 (6-ethoxyphenolato))(pentane-2,4-dionato-\k2 O,O&#x2032;)-dinickel(II),
 C38H48N4Ni2O9
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              407
_journal_page_last               409
_journal_paper_doi               10.1515/ncrs-2023-0043
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C38 H48 N4 Ni2 O9'
_chemical_formula_sum            'C38 H48 N4 Ni2 O9'
_chemical_formula_weight         822.22
_chemical_name_systematic
;
aqua(\m~2~-2,2',2''-((nitrilo)tris(ethane-2,1-diyl(nitrilo)methylylidene))
tris(6-ethoxyphenolato))(pentane-2,4-dionato-\k^2^O,O')-dinickel(II)
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                76.5677(14)
_cell_angle_beta                 83.5128(13)
_cell_angle_gamma                62.3638(14)
_cell_formula_units_Z            2
_cell_length_a                   12.3498(5)
_cell_length_b                   13.0376(6)
_cell_length_c                   13.2909(5)
_cell_measurement_reflns_used    9971
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      26.04
_cell_measurement_theta_min      2.23
_cell_volume                     1843.95(14)
_computing_cell_refinement       'Bruker SAINT [1]'
_computing_data_collection       'Bruker APEX2 [1]'
_computing_data_reduction        'Bruker SAINT [1]'
_computing_molecular_graphics    'ORTEP-III [3]'
_computing_publication_material  'SHELXL-2014/7 [2]'
_computing_structure_refinement  'SHELXL-2014/7 [2]'
_computing_structure_solution    'SHELXL-2014/7 [2]'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            51550
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.079
_diffrn_reflns_theta_min         2.137
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.082
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7034
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2016) [1]'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_description       Block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.583
_refine_diff_density_min         -0.398
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         7294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0308
_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^)+(0.0298P)^2^+1.1711P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5989
_reflns_number_total             7294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2023-0043_suppl.cif
_cod_data_source_block           Ni(EtOsaltren)(acac)
_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 built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8738 2021-04-28 16:35:53Z antanas 
;
_cod_original_cell_volume        1843.95(13)
_cod_database_code               8107454
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.789
_shelx_estimated_absorpt_t_max   0.881
_shelx_res_checksum              30733
_shelx_hkl_checksum              92217