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_2108985
_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         'C22 H24 Cu N2 O8, 4(H2 O)'
_chemical_formula_sum            'C22 H32 Cu N2 O12'
_chemical_formula_weight         580.03
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2021-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-08-18 deposited with the CCDC. 2021-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.510(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9887(7)
_cell_length_b                   6.8910(2)
_cell_length_c                   14.3405(7)
_cell_measurement_reflns_used    3907
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.5780
_cell_measurement_theta_min      4.1490
_cell_volume                     1303.00(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1158
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.988
_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    -12.00  88.00   1.00   65.91    --   18.19  77.00   0.00  100
  2  \w    -52.00  48.00   1.00   65.91    --   18.19 -77.00-120.00  100
  3  \w    -25.00  23.00   1.00   65.91    --  -18.58 -99.00  60.00   48
  4  \w     35.00  83.00   1.00   65.91    --   18.19 178.00-120.00   48
  5  \w    -55.00  62.00   1.00   65.91    --   18.19 -19.00 -30.00  117
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0537578000
_diffrn_orient_matrix_UB_12      -0.0026295000
_diffrn_orient_matrix_UB_13      0.0162152000
_diffrn_orient_matrix_UB_21      0.0000576000
_diffrn_orient_matrix_UB_22      -0.0716598000
_diffrn_orient_matrix_UB_23      0.0355133000
_diffrn_orient_matrix_UB_31      -0.0019550000
_diffrn_orient_matrix_UB_32      -0.0738856000
_diffrn_orient_matrix_UB_33      -0.0350382000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9459
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         3.820
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.903
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.77486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       needle
_exptl_crystal_F_000             606
_exptl_crystal_recrystallization_method
'Obtained directly from synthesis mother liquor'
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.382
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details
;
 Flack x determined using 1656 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4711
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0376
_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^)+(0.0502P)^2^+0.0870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0939
_reflns_Friedel_coverage         0.804
_reflns_Friedel_fraction_full    0.953
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                4234
_reflns_number_total             4711
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5107sup1.cif
_cod_data_source_block           exp_5058_sq
_cod_database_code               2108985
_publcif_datablock.id            {f38d5590-d825-4d4e-896d-cae005477b7f}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.571
_reflns_odcompleteness_completeness 99.55
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H) groups, All O(H,H) groups
2. Others
 Sof(O13)=Sof(H13D)=Sof(H13E)=1-FVAR(1)
 Sof(O12)=Sof(H12A)=Sof(H12B)=FVAR(1)
3.a Free rotating group:
 O10(H10D,H10E), O9(H9A,H9B), O11(H11A,H11B), O12(H12A,H12B), O13(H13D,H13E)
3.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), C9(H9), C14(H14)
3.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B), C15(H15A,H15B), C22(H22A,H22B)
3.d Aromatic/amide H refined with riding coordinates:
 C2(H2A), C3(H3), C6(H6), C17(H17), C20(H20), C21(H21)
3.e Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              26360
_shelx_hkl_checksum              39263
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.271
_oxdiff_exptl_absorpt_empirical_full_min 0.802
_cod_database_fobs_code 2108985