The affinity of copper(II) ions towards L-amino acids in the solid-state: a simple route towards mixed complexes
Smokrovic, Kristina; Đilović, Ivica; Matkovic-Calogovic, Dubravka; CrystEngComm  (2020) –; doi:10.1039/D0CE00687D

data_7240825
_publ_section_title
;
 The affinity of copper(II) ions towards L-amino acids in the solid-state:
 a simple route towards mixed complexes
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00687D
_journal_year                    2020
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C11 H16 Cu N4 O4, 2(H2 O)'
_chemical_formula_sum            'C11 H20 Cu N4 O6'
_chemical_formula_weight         367.85
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2019-10-07
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.03 svn.r3662 for OlexSys, GUI svn.r5945)
;
_audit_update_record
;
2020-05-13 deposited with the CCDC.	2020-07-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.199(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7066(6)
_cell_length_b                   8.1806(4)
_cell_length_c                   10.3710(6)
_cell_measurement_reflns_used    3271
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.9670
_cell_measurement_theta_min      4.4750
_cell_volume                     751.15(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_computing_structure_solution    'XS n/a (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.3426
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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     -2.00  62.00   1.00   15.00    --   25.57   0.00 -90.00   64
  2  \w     40.00 102.00   1.00   15.00    --   25.57 179.00 -30.00   62
  3  \w      5.00  63.00   1.00   15.00    --   25.57  57.00   0.00   58
  4  \w     14.00  94.00   1.00   15.00    --   25.57  57.00  60.00   80
  5  \w     53.00  99.00   1.00   15.00    --   25.57 179.00-120.00   46
  6  \w    -97.00  -7.00   1.00   15.00    --  -28.54 -57.00 120.00   90
  7  \w     -5.00  40.00   1.00   15.00    --  -28.54  57.00 -90.00   45
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0002980000
_diffrn_orient_matrix_UB_12      0.0774844000
_diffrn_orient_matrix_UB_13      0.0307455000
_diffrn_orient_matrix_UB_21      0.0653001000
_diffrn_orient_matrix_UB_22      -0.0227586000
_diffrn_orient_matrix_UB_23      0.0604493000
_diffrn_orient_matrix_UB_31      0.0464956000
_diffrn_orient_matrix_UB_32      0.0315096000
_diffrn_orient_matrix_UB_33      -0.0319882000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6231
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.990
_diffrn_reflns_theta_min         4.208
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       block
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.333
_exptl_crystal_size_mid          0.286
_exptl_crystal_size_min          0.094
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 1229 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.003(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         3261
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0334
_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^)+(0.0424P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0781
_refine_ls_wR_factor_ref         0.0815
_reflns_Friedel_coverage         0.868
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                2947
_reflns_number_total             3261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00687d2.cif
_cod_data_source_block           exp_2401
_cod_database_code               7240825
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O Cu1'
_reflns_odcompleteness_completeness 99.46
_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 C(H,H,H,H) groups, All N(H) groups,
  All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 H1B-O12_$1
 2.38 with sigma of 0.04
3. Others
 Fixed Sof: H15A(0.68113) H15B(0.68113) H15C(0.31887) H15D(0.31887)
 H13A(0.68113) H13B(0.68113) H13C(0.31887) H13D(0.31887) C14(0.68113)
 H14A(0.68113) H14B(0.68113) C14A(0.31887) H14C(0.31887) H14D(0.31887)
4.a Free rotating group:
 O2(H2A,H2B), O1(H1A,H1B)
4.b Ternary CH refined with riding coordinates:
 N11(H11), C22(H22), C12(H12)
4.c Secondary CH2 refined with riding coordinates:
 N21(H21A,H21B), C23(H23A,H23B), C15(H15A,H15B), C15(H15C,H15D), C13(H13A,
 H13B), C13(H13C,H13D), C14(H14A,H14B), C14A(H14C,H14D)
4.d Aromatic/amide H refined with riding coordinates:
 C26(H26), N23(H23), C25(H25)
;
_shelx_res_checksum              17077
_olex2_date_sample_data_collection 2017-03-19
_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 1.343
_oxdiff_exptl_absorpt_empirical_full_min 0.839