Tetranuclear Cu(ii)-chiral complexes: synthesis, characterization and biological activity
Peewasan, Krisana; Merkel, Marcel P.; Zarschler, Kristof; Stephan, Holger; Anson, Christopher E.; Powell, Annie K.; RSC Advances 9 (2019) 24087–; doi:10.1039/C9RA03586A

data_7233318
_publ_section_title
;
 Tetranuclear Cu(ii)-chiral complexes: synthesis, characterization and
 biological activity
;
_journal_issue                   42
_journal_name_full               'RSC Advances'
_journal_page_first              24087
_journal_paper_doi               10.1039/C9RA03586A
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C69.7 H76.8 Cu4 N4 O14, 2(N1 O3), C H4 O'
_chemical_formula_sum            'C70.7 H80.8 Cu4 N6 O21'
_chemical_formula_weight         1604.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2019-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-04-25 deposited with the CCDC.    2019-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.70
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.583
_cell_length_b                   21.529
_cell_length_c                   15.571
_cell_measurement_reflns_used    23210
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.79
_cell_measurement_theta_min      1.31
_cell_volume                     3535.789
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_wavelength     0.71359
_diffrn_reflns_av_R_equivalents  0.0873
_diffrn_reflns_av_unetI/netI     0.0750
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28025
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.350
_diffrn_reflns_theta_max         26.485
_diffrn_reflns_theta_min         1.899
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  0.7968
_exptl_absorpt_correction_T_min  0.5960
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            'metallic dark green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_description       block
_exptl_crystal_F_000             1662
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.732
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.003(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     935
_refine_ls_number_reflns         14367
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0710P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1200
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                10887
_reflns_number_total             14367
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03586a2.cif
_cod_data_source_block           kp78
_cod_original_cell_volume        3536.0
_cod_original_formula_sum        'C70.70 H80.80 Cu4 N6 O21'
_cod_database_code               7233318
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.804
_shelx_estimated_absorpt_t_min   0.527
_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, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O14-H14
 0.88 with sigma of 0.04
 O3-H3
 0.88 with sigma of 0.04
 O9-H9
 0.88 with sigma of 0.04
 O13-H13
 0.88 with sigma of 0.04
 C71-O71A = C71-O71B
 1.48 with sigma of 0.02
 O19A-N6A \\sim N6A-O20A
 with sigma of 0.02
 O18B-N6B \\sim O18A-N6A \\sim O19B-N6B \\sim O20B-N6B \\sim O19A-N6A \\sim
O20A-N6A
 with sigma of 0.02
 O18A-O19A \\sim O19A-O20A \\sim O20A-O18A
 with sigma of 0.02
 O18B-O19B \\sim O19B-O20B \\sim O20B-O18B
 with sigma of 0.02
3. Restrained planarity
 O18A, O19A, O20A, N6A
 with sigma of 0.1
 O18B, O19B, O20B, N6B, N6B, N6B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O18A \\sim O18B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
N6A \\sim N6B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
5. Rigid body (RIGU) restrains
 O18A, O19A, O20A, N6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: H13(0.7) C69A(0.7) H69A(0.7) H69B(0.7) H69C(0.7) O18A(0.7)
 O18B(0.3) O19A(0.7) O19B(0.3) O20A(0.7) O20B(0.3) N6A(0.7) N6B(0.3) O71A(0.5)
 H71A(0.5) O71B(0.5) H71B(0.5) H71C(0.5) H71D(0.5) H71E(0.5) H71F(0.5)
 H71G(0.5) H71H(0.5)
7.a Ternary CH refined with riding coordinates:
 C9(H9A), C26(H26), C43(H43), C60(H60)
7.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C27(H27A,H27B), C28(H28A,H28B), C44(H44A,
 H44B), C45(H45A,H45B), C61(H61A,H61B), C62(H62A,H62B)
7.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C5(H5), C7(H7), C13(H13A), C14(H14A), C15(H15), C16(H16),
 C17(H17), C20(H20), C21(H21), C22(H22), C24(H24), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C41(H41), C47(H47),
 C48(H48), C49(H49), C50(H50), C51(H51), C54(H54), C55(H55), C56(H56), C58(H58),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68)
7.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C42(H42A,H42B,H42C), C59(H59A,H59B,
 H59C), C69A(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71(H71C,H71D,H71E),
 C71(H71F,H71G,H71H)
7.e Idealised tetrahedral OH refined as rotating group:
 O71A(H71A), O71B(H71B)
;
_shelx_res_checksum              70127
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'