Coordination geometry flexibility driving supramolecular isomerism of Cu/Mo pillared-layer hybrid networks.
Moya, Marielsys; Liendo-Polanco, Gustavo R; Atencio, Reinaldo; Silva, Pedro; Henao, Jose A.; Bruno-Colmenares, Julia; Acta crystallographica Section B, Structural science, crystal engineering and materials 80 (2024) 782–792; doi:10.1107/S2052520624009934

data_2312708
_publ_section_title
;
 Coordination geometry flexibility driving supramolecular isomerism of
 Cu/Mo pillared-layer hybrid networks.
;
_journal_issue                   6
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              782
_journal_page_last               792
_journal_paper_doi               10.1107/S2052520624009934
_journal_volume                  80
_journal_year                    2024
_chemical_formula_moiety         'C40 H32 Cu4 Mo8 N8 O26'
_chemical_formula_sum            'C40 H32 Cu4 Mo8 N8 O26'
_chemical_formula_weight         2062.41
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1363(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.86409(18)
_cell_length_b                   11.2440(2)
_cell_length_c                   21.9304(3)
_cell_measurement_reflns_used    19103
_cell_measurement_temperature    100.00(14)
_cell_measurement_theta_max      29.3590
_cell_measurement_theta_min      2.5540
_cell_volume                     2671.95(7)
_computing_cell_refinement       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.75a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3196
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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      9.00  69.00   1.00    9.92    --   11.07-130.00 -30.00   60
  2  \w     13.00  76.00   1.00    9.92    --   11.07-139.00 155.00   63
  3  \w    -42.00  22.00   1.00    9.92    --  -10.68 -77.00  60.00   64
  4  \w    -85.00  14.00   1.00    9.92    --  -10.68 -37.00-180.00   99
  5  \w    -42.00  44.00   1.00    9.92    --   11.07 -77.00-150.00   86
  6  \w    -39.00 -14.00   1.00    9.92    --  -10.68  57.00 -30.00   25
  7  \w    -17.00  84.00   1.00    9.92    --   11.07  57.00   0.00  101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0008865000
_diffrn_orient_matrix_UB_12      0.0627362000
_diffrn_orient_matrix_UB_13      -0.0034408000
_diffrn_orient_matrix_UB_21      0.0282762000
_diffrn_orient_matrix_UB_22      0.0063625000
_diffrn_orient_matrix_UB_23      0.0299939000
_diffrn_orient_matrix_UB_31      0.0590435000
_diffrn_orient_matrix_UB_32      -0.0021014000
_diffrn_orient_matrix_UB_33      -0.0118066000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            32759
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.681
_diffrn_reflns_theta_min         1.862
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.458
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.643
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.75a (Rigaku Oxford Diffraction, 2022)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic light yellow'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.563
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.112
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.671
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0230
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0196P)^2^+2.9699P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0494
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4541
_reflns_number_total             5067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yv5021sup1.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 2312705--2312708.cif.'
_cod_original_cell_volume        2671.95(8)
_cod_database_code               2312708
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40H38Cu4Mo8N8O26
_chemical_oxdiff_usercomment     Y1803d_ReinaldoAtencio_IVIC
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12),
 C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20)
;
_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 2.382
_oxdiff_exptl_absorpt_empirical_full_min 0.615