Oxochlorin frameworks confining a β-hydroxyketone moiety.
Chaudhri, Nivedita; Guberman-Pfeffer, Matthew J; Zeller, Matthias; Brückner, Christian; Dalton transactions (Cambridge, England : 2003) 53 (2024) 13142–13150; doi:10.1039/d4dt01386g

data_7716640
_publ_section_title
;
 Oxochlorin frameworks confining a &#x3b2;-hydroxyketone moiety.
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13142
_journal_page_last               13150
_journal_paper_doi               10.1039/d4dt01386g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H44 N4 Ni O2, 0.0773(H2 O)'
_chemical_formula_sum            'C36 H44.15 N4 Ni O2.08'
_chemical_formula_weight         624.85
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-03-17 deposited with the CCDC.	2024-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                109.334(7)
_cell_angle_beta                 97.626(8)
_cell_angle_gamma                91.299(7)
_cell_formula_units_Z            3
_cell_length_a                   8.6985(10)
_cell_length_b                   14.5755(16)
_cell_length_c                   20.098(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      77.3575
_cell_measurement_theta_min      2.3559
_cell_volume                     2377.1(5)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2020)'
_computing_data_collection       'Apex4 v2022.1-1 (Bruker, 2022)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2020)'
_computing_structure_refinement
;  
SHELXL-2019/2 (Sheldrick, 2015a, 2019), 
SHELXLE Rev1460 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXT (Sheldrick, 2015b)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 7.4074
_diffrn_detector_type
'PhotonIII_C14 charge-integrating and photon counting pixel array'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device       'four circle diffractometer'
_diffrn_measurement_device_type  'Bruker AXS D8 Quest'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1099
_diffrn_reflns_av_unetI/netI     0.1184
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30684
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         81.161
_diffrn_reflns_theta_min         2.356
_diffrn_source                   'I-mu-S microsource X-ray tube'
_diffrn_source_current           '1.0 mA'
_diffrn_source_voltage           '50 kV'
_exptl_absorpt_coefficient_mu    1.180
_exptl_absorpt_correction_T_max  0.7544
_exptl_absorpt_correction_T_min  0.5948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_description       flake
_exptl_crystal_F_000             998.3
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.0027(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     891
_refine_ls_number_reflns         9596
_refine_ls_number_restraints     743
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.1344
_refine_ls_R_factor_gt           0.0732
_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^)+(0.1221P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1853
_refine_ls_wR_factor_ref         0.2363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5258
_reflns_number_total             9596
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01386g2.cif
_cod_data_source_block           NIMOC_OH_0m
_cod_depositor_comments
'Adding full bibliography for 7716640--7716641.cif.'
_cod_database_code               7716640
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.922
_shelx_estimated_absorpt_t_max   0.988
_shelx_res_checksum              86874
_shelx_hkl_checksum              49738