Nitric oxide generation study of unsymmetrical β-diketiminato copper(II) nitrite complexes
Chand, Kuldeep; Chu, Yu-Cheng; Wang, Tzai-Wei; Kao, Chai-Lin; Lin, Ya-Fan; Tsai, Ming-Li; Hsu, Sodio C.N.; Dalton Transactions  (2022) –; doi:10.1039/D1DT03711K

data_7709375
_publ_section_title
;
 Nitric oxide generation study of unsymmetrical \b-diketiminato copper(II)
 nitrite complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03711K
_journal_year                    2022
_chemical_formula_moiety         'C23 H30 Cl Cu N3'
_chemical_formula_sum            'C23 H30 Cl Cu N3'
_chemical_formula_weight         447.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-11-25
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2021-11-25 deposited with the CCDC.	2022-01-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.9140(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0105(7)
_cell_length_b                   15.2571(5)
_cell_length_c                   15.5984(5)
_cell_measurement_reflns_used    9669
_cell_measurement_temperature    200.01
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.96
_cell_volume                     4469.6(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      200.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            79616
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.269
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.110
_exptl_absorpt_correction_T_max  0.8424
_exptl_absorpt_correction_T_min  0.6529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1880
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.308
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         7851
_refine_ls_number_restraints     1753
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0261P)^2^+3.6556P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6752
_reflns_number_total             7851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03711k2.cif
_cod_data_source_block           d18830
_cod_database_code               7709375
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.842
_shelx_estimated_absorpt_t_min   0.653
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C38, C40
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 9.3
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim N1 \\sim N2 \\sim N3
\\sim N4 \\sim N5 \\sim N6 \\sim Cu1 \\sim Cu2 \\sim Cu3 \\sim Cl1 \\sim Cl2
\\sim Cl3: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.2
within 3.8A
4. Others
 Sof(Cu3)=Sof(Cl3)=1-FVAR(1)
 Sof(Cu2)=Sof(Cl2)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C35(H35), C38(H38)
5.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C41(H41A,H41B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C23(H23),
 C26(H26), C31(H31), C32(H32), C33(H33), C43(H43), C44(H44), C45(H45), C46(H46)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C24(H24A,H24B,H24C), C28(H28A,H28B,
 H28C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C40(H40A,
 H40B,H40C)
;
_shelx_res_checksum              82885
_shelx_hkl_checksum              97843
_olex2_submission_special_instructions 'No special instructions were received'