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_2312705
_publ_section_title
;
 Coordination geometry flexibility driving supramolecular isomerism of
 Cu/Mo pillared-layer hybrid networks.
;
_journal_coeditor_code           YV5021
_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 O16, 0.3(H2 O)'
_chemical_formula_sum            'C40 H32.6 Cu4 Mo4 N8 O16.3'
_chemical_formula_weight         1524.06
_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   mixed
_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                 103.035(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7136(12)
_cell_length_b                   23.759(3)
_cell_length_c                   19.9289(17)
_cell_measurement_reflns_used    8236
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.2320
_cell_measurement_theta_min      1.5800
_cell_volume                     4480.8(9)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Rigaku XTaLAB P200'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0996
_diffrn_reflns_av_unetI/netI     0.0987
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37915
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        24.870
_diffrn_reflns_theta_max         24.870
_diffrn_reflns_theta_min         2.152
_exptl_absorpt_coefficient_mu    3.025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64422
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'DTABSCOR program'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.259
_exptl_crystal_description       plate
_exptl_crystal_F_000             2972
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.449
_refine_diff_density_min         -1.280
_refine_diff_density_rms         0.217
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     658
_refine_ls_number_reflns         7695
_refine_ls_number_restraints     90
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0616
_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^)+(0.0802P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1680
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4828
_reflns_number_total             7695
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yv5021sup1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 2312705--2312708.cif.'
_cod_original_formula_sum        'C40 H32.60 Cu4 Mo4 N8 O16.30'
_cod_database_code               2312705
_cod_database_fobs_code          2312705
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.643
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(N7) \\sim Ueq, Uanis(C30)
\\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C37)
\\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.008 and sigma for terminal
atoms of 0.0016
Uanis(C5) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
Uanis(C20) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016
3. Others
 Fixed Sof: O1W(0.3) H1WA(0.3) H1WB(0.3)
4.a Riding coordinates:
 O1W(H1WA,H1WB)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22),
  C25(H25), C26(H26), C27(H27), C28(H28), C39(H39), C40(H40), C35(H35),
 C36(H36), C37(H37), C38(H38), C29(H29), C30(H30), C33(H33), C32(H32), C8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'