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_2108986
_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_formula_moiety         'C22 H24 Cu N2 O8'
_chemical_formula_sum            'C22 H24 Cu N2 O8'
_chemical_formula_weight         507.97
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-06-30
_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                90
_cell_angle_beta                 96.84(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.279(3)
_cell_length_b                   5.5252(9)
_cell_length_c                   17.450(3)
_cell_measurement_reflns_used    1968
_cell_measurement_temperature    298.5
_cell_measurement_theta_max      24.2000
_cell_measurement_theta_min      4.1020
_cell_volume                     1079.7(4)
_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 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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298.5
_diffrn_detector_area_resol_mean 16.1158
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.867
_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     44.00  84.00   1.00   76.78    --   16.31  57.00  30.00   40
  2  \w      5.00  80.00   1.00   76.78    --   16.31  57.00   0.00   75
  3  \w    -25.00  55.00   1.00   76.78    --   16.31 -99.00 -90.00   80
  4  \w     35.00  89.00   1.00   76.78    --   16.31 178.00 -90.00   54
  5  \w    -13.00  15.00   1.00   76.78    --   16.31  19.00 -30.00   28
  6  \w    -77.00 -43.00   1.00   76.78    --  -16.78 -57.00   0.00   34
  7  \w     -8.00  22.00   1.00   76.78    --  -16.78 -99.00 120.00   30
  8  \w    -38.00  47.00   1.00   76.78    --  -16.78  77.00  90.00   85
  9  \w     20.00  45.00   1.00   76.78    --  -16.78  77.00  60.00   25
 10  \w    -24.00   7.00   1.00   76.78    --  -16.78 -99.00  60.00   31
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0935
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.867
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10344
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.867
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.334
_diffrn_reflns_theta_min         3.639
_exptl_absorpt_coefficient_mu    1.065
_exptl_absorpt_correction_T_max  0.73189
_exptl_absorpt_correction_T_min  0.72401
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.562
_exptl_crystal_description       needle
_exptl_crystal_F_000             526
_exptl_crystal_preparation
'Heating an acquos solution of the hydrateted form.'
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Water/NH3'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.559
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2576
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0626P)^2^+0.0382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1250
_refine_ls_wR_factor_ref         0.1515
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1577
_reflns_number_total             2576
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lo5107sup1.cif
_cod_data_source_block           exp_4899_p1
_cod_database_code               2108986
_publcif_datablock.id            {caa61a4b-dfaf-40a2-a10f-b1024da14b1e}
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.949
_shelx_estimated_absorpt_t_min   0.901
_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
2.a Ternary CH refined with riding coordinates:
 N2(H2), C14(H14)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C22(H22A,H22B)
2.c Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C20(H20)
2.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C)
;
_shelx_res_checksum              97589
_shelx_hkl_checksum              38128
_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
;
_cod_database_fobs_code 2108986