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_2312707
_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 Mo4 N8 O15, 0.4[H2O]'
_chemical_formula_sum            'C40 H32.8 Cu4 Mo4 N8 O15.4'
_chemical_formula_weight         1509.86
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6940(3)
_cell_length_b                   9.0285(2)
_cell_length_c                   21.3258(4)
_cell_measurement_reflns_used    7937
_cell_measurement_temperature    100.0(5)
_cell_measurement_theta_max      29.2320
_cell_measurement_theta_min      2.5520
_cell_volume                     2251.56(9)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3196
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -90.00  28.00   1.00    2.44    --  -10.68 -20.00 148.00  118
  2  \w     21.00  87.00   1.00    2.44    --   11.15-154.00 148.00   66
  3  \w    -43.00  21.00   1.00    2.44    --  -10.68  77.00 -60.00   64
  4  \w    -42.00 -17.00   1.00    2.44    --  -10.68 -77.00  60.00   25
;
_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      -0.0590858000
_diffrn_orient_matrix_UB_12      0.0123999000
_diffrn_orient_matrix_UB_13      0.0054388000
_diffrn_orient_matrix_UB_21      0.0117645000
_diffrn_orient_matrix_UB_22      0.0161403000
_diffrn_orient_matrix_UB_23      0.0318956000
_diffrn_orient_matrix_UB_31      0.0071780000
_diffrn_orient_matrix_UB_32      0.0758730000
_diffrn_orient_matrix_UB_33      -0.0076762000
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0258
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15114
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.585
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.007
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.760
_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 intense red'
_exptl_crystal_density_diffrn    2.227
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.681
_refine_diff_density_min         -0.896
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2299
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0385P)^2^+4.4440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0712
_refine_ls_wR_factor_ref         0.0763
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2015
_reflns_number_total             2299
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yv5021sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 2312705--2312708.cif.'
_cod_original_formula_sum        'C40 H32.80 Cu4 Mo4 N8 O15.40'
_cod_database_code               2312707
_cod_database_fobs_code          2312707
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C40H32Cu4Mo4N8O16
_chemical_oxdiff_usercomment     R1803d_ReinaldoAtencio_IVIC_rep
_shelx_estimated_absorpt_t_max   0.696
_shelx_estimated_absorpt_t_min   0.437
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 Mo1-O3 \\sim Mo1A-O3A
 with sigma of 0.02
 O4-O3 \\sim O4A-O3A
 with sigma of 0.04
 O1-O3 \\sim O1-O3A
 with sigma of 0.04
 O2-O3 \\sim O2-O3A
 with sigma of 0.04
 Mo1-O1 \\sim Mo1A-O1
 with sigma of 0.02
 Mo1-O4 \\sim Mo1A-O4A
 with sigma of 0.02
 O1-O4 \\sim O1-O4A
 with sigma of 0.04
 O2-O4 \\sim O2-O4A
 with sigma of 0.04
 Mo1-O2 \\sim Mo1A-O2
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O3) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(O3) = Uanis(O3A)
Uanis(O4) = Uanis(O4A)
Uanis(Mo1) = Uanis(Mo1A)
4. Others
 Sof(O4)=Sof(Mo1A)=1-FVAR(1)
 Sof(Mo1)=Sof(O4A)=FVAR(1)
 Fixed Sof: O3(0.25) O3A(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C9(H9), C8(H8), C1(H1), C2(H2), C4(H4), C7(H7)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 2.986
_oxdiff_exptl_absorpt_empirical_full_min 0.692