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_7709379
_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 Cu N4 O2, 1.779(C0.562 H1.124 Cl1.124)'
_chemical_formula_sum            'C24 H32 Cl2 Cu N4 O2'
_chemical_formula_weight         542.97
_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
_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                 99.2350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.0788(10)
_cell_length_b                   10.1901(3)
_cell_length_c                   15.8411(5)
_cell_measurement_reflns_used    9862
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.004
_cell_measurement_theta_min      2.412
_cell_volume                     5270.4(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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            49501
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.356
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.059
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5119
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1259 before and 0.0737 after correction.
The Ratio of minimum to maximum transmission is 0.6869.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.798
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         9249
_refine_ls_number_restraints     1964
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0620P)^2^+7.2801P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7340
_reflns_number_total             9249
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03711k2.cif
_cod_data_source_block           l1cu(o2n)
_cod_database_code               7709379
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.939
_shelx_estimated_absorpt_t_min   0.785
_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. Restrained distances
 C48-Cl3 \\sim C49-Cl5
 with sigma of 0.02
 C48-Cl4 \\sim C49-Cl6
 with sigma of 0.02
 Cl3-Cl4 \\sim Cl5-Cl6
 with sigma of 0.04
3. Rigid bond restraints
 O4, N5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 13.5
 O2, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 14.5
 O1, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 5.5
 Cu1, O1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 8.3
 Cu1, O2
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 8.4
 Cu2, O3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 7.4
 Cu2, O4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 9.5
4. 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 C47 \\sim C48 \\sim C49
\\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim
O1 \\sim O2 \\sim O3 \\sim O4 \\sim Cl1 \\sim Cl2 \\sim Cl3 \\sim Cl4 \\sim Cl5
\\sim Cl6 \\sim Cu1 \\sim Cu2: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
Uanis(Cl1) \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(Cl3) \\sim Ueq, Uanis(Cl4)
\\sim Ueq, Uanis(Cl5) \\sim Ueq, Uanis(Cl6) \\sim Ueq: with sigma of 0.008 and
sigma for terminal atoms of 0.008
5. Others
 Sof(Cl5)=Sof(Cl6)=Sof(C49)=Sof(H49A)=Sof(H49B)=1-FVAR(1)
 Sof(Cl3)=Sof(Cl4)=Sof(C48)=Sof(H48A)=Sof(H48B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C35(H35), C38(H38)
6.b Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C41(H41A,H41B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B)
6.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)
6.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              49134
_shelx_hkl_checksum              13308
_olex2_submission_special_instructions 'No special instructions were received'