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_7233317
_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_absolute_configuration rmad
_chemical_formula_moiety         'C70 H78 Cu4 N4 O14, 2(N O3), C H4 O'
_chemical_formula_sum            'C71 H82 Cu4 N6 O21'
_chemical_formula_weight         1609.58
_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
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_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                 94.833(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6198(7)
_cell_length_b                   21.4213(14)
_cell_length_c                   15.6347(12)
_cell_measurement_reflns_used    23063
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.76
_cell_measurement_theta_min      1.31
_cell_volume                     3544.1(4)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.144.0 (STOE, 2018)'
_computing_data_reduction        'X-Area Integrate 1.73.0.0 (STOE, 2018)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'image plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0652
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29165
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         26.731
_diffrn_reflns_theta_min         1.616
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_T_max  0.9928
_exptl_absorpt_correction_T_min  0.9832
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-Area LANA 1.72.3.0 (STOE, 2018)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       block
_exptl_crystal_F_000             1668
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.618
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 3909 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.010(7)
_refine_ls_extinction_coef       0.0010(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         14517
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0478P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.881
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.928
_reflns_number_gt                10173
_reflns_number_total             14517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra03586a2.cif
_cod_data_source_block           kp38
_cod_database_code               7233317
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.673
_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 O(H) groups
2. Restrained distances
 O3-H3
 0.88 with sigma of 0.04
 H3-O20
 1.85 with sigma of 0.04
 O9-H9
 0.88 with sigma of 0.04
 O13-H13
 0.88 with sigma of 0.04
 O14-H14
 0.88 with sigma of 0.04
 O71A-C71A = O71B-C71B
 1.48 with sigma of 0.02
 O20-H71A
 1.9 with sigma of 0.04
 H71E-O19
 2.05 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
O71B \\sim C71A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 O18, O19, O20, N6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O71A(0.5) H71A(0.5) C71A(0.5) H71B(0.5) H71C(0.5) H71D(0.5)
 C71B(0.5) H71E(0.5) H71F(0.5) H71G(0.5) O71B(0.5) H71H(0.5)
6.a Ternary CH refined with riding coordinates:
 C9(H9A), C26(H26), C43(H43), C60(H60)
6.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)
6.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)
6.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C25(H25A,H25B,H25C), C42(H42A,H42B,H42C), C59(H59A,H59B,
 H59C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C), C71A(H71B,H71C,H71D),
 C71B(H71E,H71F,H71G)
6.e Idealised tetrahedral OH refined as rotating group:
 O71A(H71A), O71B(H71H)
;
_shelx_res_checksum              30798
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'