Synthesis, structural and electrochemical properties of a new family of amino-acid-based coordination complexes
Rey, Juan Manuel; Movilla, Federico; Suárez, Sebastián Angel; Di Salvo, Florencia; Acta Crystallographica Section B 78 (2022) –; doi:10.1107/S2052520622003912

data_2108987
_publ_section_title
;
 Synthesis, structural and electrochemical properties of a new family of
 amino-acid-based coordination complexes
;
_journal_issue                   '3 Part 2'
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2052520622003912
_journal_volume                  78
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C34 H34 Cu N2 O9'
_chemical_formula_sum            'C34 H34 Cu N2 O9'
_chemical_formula_weight         678.17
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-07-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-08-18 deposited with the CCDC. 2021-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                91.685(11)
_cell_angle_beta                 97.664(7)
_cell_angle_gamma                112.798(8)
_cell_formula_units_Z            1
_cell_length_a                   7.2450(17)
_cell_length_b                   7.2510(12)
_cell_length_c                   16.014(3)
_cell_measurement_reflns_used    9181
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.496
_cell_measurement_theta_min      2.900
_cell_volume                     765.6(3)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'MXCuBE (Gabadinho et al., 2010)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 5.814
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  mx2_info_2019
_diffrn_measurement_method       'shuterless \f scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.79986
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            7949
_diffrn_reflns_point_group_measured_fraction_full 0.909
_diffrn_reflns_point_group_measured_fraction_max 0.894
_diffrn_reflns_theta_full        27.496
_diffrn_reflns_theta_max         27.496
_diffrn_reflns_theta_min         2.900
_diffrn_source                   LNLS-MX2
_exptl_absorpt_coefficient_mu    1.061
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.779676
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       plate
_exptl_crystal_F_000             353
_exptl_crystal_recrystallization_method 'Gel crystallization'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.333
_refine_diff_density_min         -0.822
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 1962 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.012(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         4427
_refine_ls_number_restraints     165
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0613
_refine_ls_R_factor_gt           0.0600
_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^)+(0.1244P)^2^+0.2776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1570
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.942
_reflns_Friedel_fraction_full    0.881
_reflns_Friedel_fraction_max     0.867
_reflns_number_gt                4293
_reflns_number_total             4427
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5107sup1.cif
_cod_data_source_block           cu_phepip
_cod_database_code               2108987
_publcif_datablock.id            {4ff6c69e-c9e6-4a9c-8ee5-eb70ec225d5b}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.816
_exptl_absorpt_special_details
;
_exptl_absorpt_correction_T_min and _exptl_absorpt_correction_T_max
from ABSORP.cbf, the absorption factors used by XDS.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained planarity
 C1, C4, C11, C16, C19, C20
 with sigma of 0.1
 C2, C14, C21, C25, C31, C33
 with sigma of 0.1
 C8, C10, C12, C22, C28, C34
 with sigma of 0.1
 C3, C7, C15, C23, C26, C32
 with sigma of 0.1
3. Uiso/Uaniso restraints and constraints
C1 \\sim C4 \\sim C11 \\sim C16 \\sim C19 \\sim C20: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 1.7A
C2 \\sim C14 \\sim C21 \\sim C25 \\sim C31 \\sim C33: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 1.7A
C3 \\sim C7 \\sim C15 \\sim C23 \\sim C26 \\sim C32: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 1.7A
C8 \\sim C10 \\sim C12 \\sim C22 \\sim C28 \\sim C34: within 1.7A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 1.7A
Cu1 \\sim O2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.01
4.a Rotating group:
 O2(H2A,H2B)
4.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C6(H6), C17(H17)
4.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C13(H13A,H13B), C18(H18A,H18B), C24(H24A,H24B), C27(H27A,H27B),
 C29(H29A,H29B)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2C), C3(H3), C7(H7), C11(H11), C12(H12), C15(H15), C16(H16), C19(H19),
 C21(H21), C22(H22), C23(H23), C25(H25), C31(H31), C32(H32), C33(H33), C34(H34)
;
_shelx_res_checksum              26987
_shelx_hkl_checksum              20009
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 5
_publcif_info_exptl_table_use_headnotes n
_cod_database_fobs_code 2108987