Interplay of Isomorphs and Polymorphs of Amidino-Copper(II) Complexes with Different Halides
Yamba, Zaina; Peoble, Anna; Novikov, Egor; Castañeda, Raúl; Timofeeva, Tatiana; Crystals 14 (2024) 319–; doi:10.3390/cryst14040319

data_1571378
_publ_section_title
;
 Interplay of Isomorphs and Polymorphs of Amidino-Copper(II) Complexes
 with Different Halides
;
_journal_issue                   4
_journal_name_full               Crystals
_journal_page_first              319
_journal_paper_doi               10.3390/cryst14040319
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C2 F3 O2, C5 H7 N4'
_chemical_formula_sum            'C7 H7 F3 N4 O2'
_chemical_formula_weight         236.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-28
_audit_creation_method
;
Olex2 1.5-beta
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.187(18)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   5.0459(9)
_cell_length_b                   9.373(2)
_cell_length_c                   9.5454(18)
_cell_measurement_reflns_used    1858
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.6890
_cell_measurement_theta_min      2.1410
_cell_volume                     448.82(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-beta (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    101.26 180.26   0.50   40.01    --   18.00  73.75  94.26  158
  2  \w    101.26 180.26   0.50   40.01    --   18.00  73.75 134.26  158
  3  \w    101.26 180.26   0.50   40.01    --   18.00  73.75 174.26  158
  4  \w    101.26 176.26   0.50   40.01    --   14.00  73.75-145.74  150
  5  \w    101.26 176.26   0.50   40.01    --   14.00  73.75-105.74  150
  6  \w    101.26 176.26   0.50   40.01    --   14.00  73.75 -65.74  150
  7  \w    101.26 180.26   0.50   40.01    --   18.00  73.75 -25.74  158
  8  \w    101.26 180.26   0.50   40.01    --   18.00  73.75 -85.74  158
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0150294000
_diffrn_orient_matrix_UB_12      -0.0743050000
_diffrn_orient_matrix_UB_13      -0.0129274000
_diffrn_orient_matrix_UB_21      -0.0211367000
_diffrn_orient_matrix_UB_22      0.0133069000
_diffrn_orient_matrix_UB_23      -0.0735317000
_diffrn_orient_matrix_UB_31      0.1388386000
_diffrn_orient_matrix_UB_32      -0.0057537000
_diffrn_orient_matrix_UB_33      -0.0044207000
_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  0.0703
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3358
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.668
_diffrn_reflns_theta_max         24.668
_diffrn_reflns_theta_min         2.146
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.171
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36270
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_description       needle
_exptl_crystal_F_000             240
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         806
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0665
_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^)+(0.1167P)^2^+0.1154P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.2204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                537
_reflns_number_total             806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Crystals-CIFS.cif
_cod_data_source_block           1
_cod_original_cell_volume        448.83(15)
_cod_database_code               1571378
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         C4N4F3O2
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.951
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 N2-H2B \\sim N2-H2A
 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2)
;
_shelx_res_checksum              53462
_shelx_hkl_checksum              89061
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 4.231
_oxdiff_exptl_absorpt_empirical_full_min 0.576