Unprecedented copper(ii) coordination induced nucleophilic cleavage of a quinoxaline heterocycle: structural and computational studies
Bandopadhyay, Nilaj; Joshi, Mayank; Armaković, Stevan; Armaković, Sanja J.; Das, Hari Sankar; Roy Choudhury, Angshuman; Biswas, Bhaskar; CrystEngComm 23 (2021) 5078–5086; doi:10.1039/D1CE00569C

data_7243043
_publ_section_title
;
 Unprecedented copper(ii) coordination induced nucleophilic cleavage of a
 quinoxaline heterocycle: structural and computational studies
;
_journal_issue                   29
_journal_name_full               CrystEngComm
_journal_page_first              5078
_journal_page_last               5086
_journal_paper_doi               10.1039/D1CE00569C
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C24 H22 Cu N2 O4, 2(Cl O4)'
_chemical_formula_sum            'C24 H22 Cl2 Cu N2 O12'
_chemical_formula_weight         664.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-06-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2021-06-05 deposited with the CCDC.	2021-06-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.846(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.6654(4)
_cell_length_b                   12.3371(5)
_cell_length_c                   14.5545(7)
_cell_measurement_reflns_used    1625
_cell_measurement_temperature    298.0(2)
_cell_measurement_theta_max      24.4880
_cell_measurement_theta_min      3.2620
_cell_volume                     1366.59(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.0(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -64.00 118.00   0.50   10.00    --   29.89  54.00  90.00  364
  2  \w     -3.00  30.00   0.50   10.00    --   29.89  54.00-180.00   66
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.895
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7341
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         32.711
_diffrn_reflns_theta_min         2.819
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97837
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         4500
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0993
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+0.1707P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1398
_refine_ls_wR_factor_ref         0.1813
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2648
_reflns_number_total             4500
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00569c2.cif
_cod_data_source_block           cuclo4_nl1_rt
_cod_depositor_comments
'Adding full bibliography for 7243042--7243043.cif.'
_cod_database_code               7243043
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.741
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C8(H8), C4(H4), C12(H12), C9(H9), C3(H3), C10(H10), C2(H2), C11(H11)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;