An original 3D coordination polymer constructed from trinuclear nodes and tetracarboxylato spacers
Dinca, Alina S.; Dogaru, Andreea; Ion, Adrian E.; Nica, Simona; Dumitrescu, Dan; Shova, Sergiu; Lloret, Francesc; Julve, Miguel; Andruh, Marius; CrystEngComm 23 (2021) 1332–1335; doi:10.1039/D0CE01667E

data_7241823
_publ_section_title
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 An original 3D coordination polymer constructed from trinuclear nodes and
 tetracarboxylato spacers
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              1332
_journal_page_last               1335
_journal_paper_doi               10.1039/D0CE01667E
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         '0.13(C912 H1080 Cu96 N192 O288)'
_chemical_formula_sum            'C114 H135 Cu12 N24 O36'
_chemical_formula_weight         3179.93
_space_group_crystal_system      cubic
_space_group_IT_number           197
_space_group_name_Hall           'I 2 2 3'
_space_group_name_H-M_alt        'I 2 3'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-11-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-15 deposited with the CCDC.	2020-12-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.336(4)
_cell_length_b                   36.336(4)
_cell_length_c                   36.336(4)
_cell_measurement_reflns_used    53672
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.796
_cell_measurement_theta_min      1.104
_cell_volume                     47975(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Arinax MD2S/Pilatus 6M, XRD2 beamline'
_diffrn_measurement_method       'rotating crystal'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            219765
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        22.796
_diffrn_reflns_theta_max         22.796
_diffrn_reflns_theta_min         1.104
_exptl_absorpt_coefficient_mu    1.045
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    0.881
_exptl_crystal_description       prism
_exptl_crystal_F_000             12984
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.25(2)
_refine_ls_extinction_coef       0.00003(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         11372
_refine_ls_number_restraints     434
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0753
_refine_ls_R_factor_gt           0.0673
_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^)+(0.1544P)^2^+45.6318P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1939
_refine_ls_wR_factor_ref         0.2087
_reflns_Friedel_coverage         0.896
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9839
_reflns_number_total             11372
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01667e2.cif
_cod_data_source_block           ad_mof_o22_c2
_cod_depositor_comments          'Adding full bibliography for 7241823.cif.'
_cod_original_cell_volume        47975(17)
_cod_database_code               7241823
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0.75(2)
 0.25(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C9X-C8X = C8-C9 = C16X-C12X = C16-C12 = C11-C17 = C11X-C17X
 1.5 with sigma of 0.01
 C23X-C24X = C23-C24 = C25-C21 = C25X-C21X = C19X-C26X = C19-C26
 1.5 with sigma of 0.01
 N7-C25 = N7X-C25X = N5-C24 = N5X-C24X = N3-C27 = N3X-C27X = N1-C4 = N1X-C4X
 1.27 with sigma of 0.001
 N1X-C4X = N1-C4
 1.4 with sigma of 0.01
 N7-C35 = N7X-C35X
 1.4 with sigma of 0.01
 N3X-C27X = N3-C27
 1.4 with sigma of 0.01
 N1X-C4X = N1-C4 = N7X-C35X = N7-C35 = N3-C27 = N3X-C27X = N5-C31 = N5X-C31X
 1.4 with sigma of 0.01
 C28X-C27X = C27-C28 = C35X-C36X = C35-C36 = C31X-C32X = C32-C31 = C5X-C4X =
 C4-C5
 1.46 with sigma of 0.01
 N2X-C7X \\sim N2-C7 \\sim N2X-C6X \\sim N2-C6 \\sim N6X-C33X \\sim N6-C34
\\sim N6X-C34X \\sim N6-C33 ~
 N4X-C29X \\sim N4-C29 \\sim N4X-C30X \\sim N4-C30 \\sim N8X-C38X \\sim N8-C38
\\sim N8X-C37X \\sim N8-C37
 with sigma of 0.01
 N7X-C25X \\sim N7-C25 \\sim N3X-C27X \\sim N3-C27 \\sim N1X-C3X \\sim N1-C3
 with sigma of 0.01
 C28X-C27X \\sim C31X-C32 \\sim C36-C35X \\sim C5X-C4X
 with sigma of 0.01
 O9-C16 \\sim O9X-C16X \\sim O8-C16 \\sim O8X-C16X \\sim O7-C15 \\sim O7X-C15X
\\sim O6-C15 \\sim O6X-C15X
 \\sim O2X-C17X \\sim O2-C17 \\sim O3X-C17X \\sim O3-C17 \\sim O5X-C8X \\sim
O5-C8 \\sim O4-C8 \\sim O4X-C8X
 with sigma of 0.01
 Cu2X-O10X \\sim Cu2-O10 \\sim Cu2X-O4X \\sim Cu2-O4 \\sim Cu4X-O12X \\sim
Cu4-O12 \\sim Cu3X-O11X ~
 Cu3-O11 \\sim Cu1-O1 \\sim Cu1X-O1X
 with sigma of 0.01
 Cu3-N6 \\sim Cu3X-N6X \\sim Cu2X-N4X \\sim Cu2-N4 \\sim Cu1-N2 \\sim Cu1X-N2X
\\sim Cu4X-N8X \\sim Cu4-N8
 with sigma of 0.01
 Cu4X-N7X \\sim Cu4-N7 \\sim Cu3-N5 \\sim Cu3X-N5X \\sim Cu2-N4 \\sim Cu2X-N4X
\\sim Cu1-N1 \\sim Cu1X-N1X
 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cu1X) = Uanis(Cu3X) = Uanis(Cu2X) = Uanis(Cu4) = Uanis(Cu2) = Uanis(Cu4X)
= Uanis(Cu3) = Uanis(Cu1)
Uiso(N3) = Uiso(N3X) = Uiso(N7) = Uiso(N7X) = Uiso(N5) = Uiso(N5X) = Uiso(N1X)
= Uiso(N1)
Uiso(N4X) = Uiso(N4) = Uiso(N8X) = Uiso(N8) = Uiso(N6) = Uiso(N6X) = Uiso(N2) =
Uiso(N2X)
Uiso(O11) = Uiso(O11X) = Uiso(O12) = Uiso(O12X) = Uiso(O10X) = Uiso(O10)
Uiso(O2X) = Uiso(O2) = Uiso(O3X) = Uiso(O3) = Uiso(O4X) = Uiso(O4) = Uiso(O5X)
= Uiso(O5) = Uiso(O6X) = Uiso(O6) = Uiso(O7X) = Uiso(O7) = Uiso(O8X) = Uiso(O8)
= Uiso(O9X) = Uiso(O9)
Uiso(O1X) = Uiso(O1)
Uiso(C23) = Uiso(C21) = Uiso(C20) = Uiso(C19) = Uiso(C18) = Uiso(C18X) =
Uiso(C23X) = Uiso(C21X) = Uiso(C20X) = Uiso(C19X) = Uiso(C22) = Uiso(C22X)
Uiso(C13X) = Uiso(C14X) = Uiso(C9X) = Uiso(C10X) = Uiso(C11X) = Uiso(C12X) =
Uiso(C13) = Uiso(C14) = Uiso(C9) = Uiso(C10) = Uiso(C11) = Uiso(C12)
Uiso(C24X) = Uiso(C24) = Uiso(C25X) = Uiso(C25) = Uiso(C26) = Uiso(C26X)
Uiso(C16X) = Uiso(C16) = Uiso(C15) = Uiso(C15X) = Uiso(C8) = Uiso(C8X) =
Uiso(C17) = Uiso(C17X)
Uiso(C38X) = Uiso(C38) = Uiso(C37X) = Uiso(C37) = Uiso(C30X) = Uiso(C29X) =
Uiso(C29) = Uiso(C30) = Uiso(C6) = Uiso(C6X) = Uiso(C7) = Uiso(C7X) =
Uiso(C33X) = Uiso(C33) = Uiso(C34) = Uiso(C34X)
Uiso(C35X) = Uiso(C35) = Uiso(C36X) = Uiso(C36) = Uiso(C27X) = Uiso(C27) =
Uiso(C28) = Uiso(C28X) = Uiso(C32X) = Uiso(C32) = Uiso(C31X) = Uiso(C31) =
Uiso(C2) = Uiso(C4) = Uiso(C4X) = Uiso(C5) = Uiso(C5X)
5. Others
 Fixed Sof: Cu1(0.5) Cu2(0.5) Cu3(0.5) Cu4(0.5) O1(0.5) O2(0.5) O3(0.5)
 O4(0.5) O5(0.5) O6(0.5) O7(0.5) O8(0.5) O9(0.5) O10(0.5) O11(0.5) O12(0.5)
 N1(0.5) N2(0.5) N3(0.5) N4(0.5) N5(0.5) N6(0.5) N7(0.5) N8(0.5) C17(0.5)
 C13(0.5) H13(0.5) C14(0.5) C9(0.5) C10(0.5) H10(0.5) C11(0.5) C12(0.5)
 C16(0.5) C8(0.5) C29(0.5) H29A(0.5) H29B(0.5) H29C(0.5) C30(0.5) H30A(0.5)
 H30B(0.5) H30C(0.5) C27(0.5) H27(0.5) C26(0.5) H26(0.5) C35(0.5) H35A(0.5)
 H35B(0.5) C37(0.5) H37A(0.5) H37B(0.5) H37C(0.5) C24(0.5) H24(0.5) C31(0.5)
 H31A(0.5) H31B(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C6(0.5) H6A(0.5)
 H6B(0.5) H6C(0.5) C5(0.5) H5A(0.5) H5B(0.5) C4(0.5) H4A(0.5) H4B(0.5) C2(0.5)
 C1(0.5) C3(0.5) H3(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C15(0.5) C34(0.5)
 H34A(0.5) H34B(0.5) H34C(0.5) C38(0.5) H38A(0.5) H38B(0.5) H38C(0.5) C36(0.5)
 H36A(0.5) H36B(0.5) C28(0.5) H28A(0.5) H28B(0.5) C23(0.5) C22(0.5) C21(0.5)
 C20(0.5) C19(0.5) C18(0.5) C25(0.5) H25(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 Cu1X(0.5) Cu2X(0.5) Cu3X(0.5) Cu4X(0.5) O1X(0.5) O2X(0.5) O3X(0.5) O4X(0.5)
 O5X(0.5) O6X(0.5) O7X(0.5) O8X(0.5) O9X(0.5) O10X(0.5) O11X(0.5) O12X(0.5)
 N1X(0.5) N2X(0.5) N3X(0.5) N4X(0.5) N5X(0.5) N6X(0.5) N7X(0.5) N8X(0.5)
 C17X(0.5) C25X(0.5) H25X(0.5) C32X(0.5) H32C(0.5) H32D(0.5) C2X(0.5) C3X(0.5)
 H3X(0.5) C5X(0.5) H5XA(0.5) H5XB(0.5) C7X(0.5) H7XA(0.5) H7XB(0.5) H7XC(0.5)
 C6X(0.5) H6XA(0.5) H6XB(0.5) H6XC(0.5) C15X(0.5) C13X(0.5) H13X(0.5) C14X(0.5)
 C9X(0.5) C10X(0.5) H10X(0.5) C11X(0.5) C12X(0.5) C33X(0.5) H33D(0.5) H33E(0.5)
 H33F(0.5) C34X(0.5) H34D(0.5) H34E(0.5) H34F(0.5) C37X(0.5) H37D(0.5)
 H37E(0.5) H37F(0.5) C38X(0.5) H38D(0.5) H38E(0.5) H38F(0.5) C16X(0.5)
 C24X(0.5) H24X(0.5) C36X(0.5) H36C(0.5) H36D(0.5) C8X(0.5) C29X(0.5) H29D(0.5)
 H29E(0.5) H29F(0.5) C27X(0.5) H27X(0.5) C28X(0.5) H28C(0.5) H28D(0.5)
 C30X(0.5) H30D(0.5) H30E(0.5) H30F(0.5) C26X(0.5) H26X(0.5) C18X(0.5)
 C23X(0.5) C22X(0.5) C21X(0.5) C20X(0.5) C19X(0.5) C35X(0.5) H35C(0.5)
 H35D(0.5) C31X(0.5) H31C(0.5) H31D(0.5) C4X(0.5) H4XA(0.5) H4XB(0.5) C1X(0.5)
6.a Riding coordinates:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C37(H37A,H37B,H37C), C33(H33A,H33B,
 H33C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C34(H34A,H34B,H34C), C38(H38A,H38B,
 H38C), C7X(H7XA,H7XB,H7XC), C6X(H6XA,H6XB,H6XC), C33X(H33D,H33E,H33F),
 C34X(H34D,H34E,H34F), C37X(H37D,H37E,H37F), C38X(H38D,H38E,H38F), C29X(H29D,
 H29E,H29F), C30X(H30D,H30E,H30F)
6.b Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C31(H31A,H31B), C5(H5A,H5B), C4(H4A,H4B), C36(H36A,H36B),
 C28(H28A,H28B), C32(H32A,H32B), C32X(H32C,H32D), C5X(H5XA,H5XB), C36X(H36C,
 H36D), C28X(H28C,H28D), C35X(H35C,H35D), C31X(H31C,H31D), C4X(H4XA,H4XB)
6.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C10(H10), C27(H27), C26(H26), C24(H24), C3(H3), C25(H25),
 C25X(H25X), C3X(H3X), C13X(H13X), C10X(H10X), C24X(H24X), C27X(H27X),
 C26X(H26X)
6.d Fitted hexagon refined as free rotating group:
 C13(C14,C9,C10,C11,C12), C23(C22,C21,C20,C19,C18), C13X(C14X,C9X,C10X,C11X,
 C12X), C18X(C23X,C22X,C21X,C20X,C19X)
;
_shelx_res_checksum              60581
_shelx_fab_checksum              79013
_olex2_submission_special_instructions 'No special instructions were received'