Nitroaromatic-detecting zinc and cadmium coordination polymers with methyl-substituted aliphatic dicarboxylate and 4,4′-dipyridylamine ligands and diverse topologies
Contejean, Zaria I.; LaDuca, Robert L.; Journal of Solid State Chemistry 266 (2018) 44–53; doi:10.1016/j.jssc.2018.06.034

data_1560781
_publ_section_title
;
 Nitroaromatic-detecting zinc and cadmium coordination polymers with
 methyl-substituted aliphatic dicarboxylate and 4,4&#x2032;-dipyridylamine
 ligands and diverse topologies
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              44
_journal_page_last               53
_journal_paper_doi               10.1016/j.jssc.2018.06.034
_journal_volume                  266
_journal_year                    2018
_chemical_formula_moiety         '2(C68 H76 Cd4 N12 O16)'
_chemical_formula_sum            'C136 H152 Cd8 N24 O32'
_chemical_formula_weight         3534.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.0114(15)
_cell_length_b                   24.6279(19)
_cell_length_c                   28.424(2)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.90
_cell_measurement_theta_min      2.19
_cell_volume                     14008.4(18)
_computing_cell_refinement       'APEX2 (BRUKER, V2012.10-0, 2012)'
_computing_data_collection       'COSMO (BRUKER, V1.61, 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_computing_structure_solution
'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)'
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1339
_diffrn_reflns_av_unetI/netI     0.1245
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            115016
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.447
_diffrn_reflns_theta_min         1.094
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.274
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6644
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0898 before and 0.0841 after correction. The Ratio of minimum to maximum transmission is 0.8916. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_description       block
_exptl_crystal_F_000             7104
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.472
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(6)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     772
_refine_ls_number_reflns         25838
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0688
_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^)+(0.0672P)^2^+14.0622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1852
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                14829
_reflns_number_total             25838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            0cd33dmgdpainversiontwinfinal.cif
_cod_data_source_block           pbca3
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the built-in table derived
from the CIF Core dictionary named 'cif_core.dic' version 2.4.5 last
updated on 2014-11-21.

Automatic conversion script
Id: cif_fix_values 8369 2020-08-20 11:38:08Z andrius 
;
_cod_original_cell_volume        14008.4(19)
_cod_database_code               1560781
_shelx_estimated_absorpt_t_max   0.883
_shelx_estimated_absorpt_t_min   0.784
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.60(6)
 0.40(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C93-C94
 1.55 with sigma of 0.02
 C93-C96
 1.55 with sigma of 0.02
 C93-C97
 1.55 with sigma of 0.02
 C93-C98
 1.55 with sigma of 0.02
 C92-C93
 1.55 with sigma of 0.02
 C153-C152
 1.55 with sigma of 0.02
 C153-C154
 1.55 with sigma of 0.02
 C153-C157
 1.55 with sigma of 0.02
 C153-C156
 1.55 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(C45) = Uanis(N13) = Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44) =
Uanis(N14) = Uanis(C48) = Uanis(C47) = Uanis(C46) = Uanis(N15) = Uanis(C49) =
Uanis(C50)
Uanis(N10) = Uanis(C37) = Uanis(C38) = Uanis(C36) = Uanis(C40) = Uanis(C39) =
Uanis(N11) = Uanis(C33) = Uanis(C34) = Uanis(C32) = Uanis(C31) = Uanis(N12) =
Uanis(C35)
Uanis(C70) = Uanis(N21) = Uanis(C66) = Uanis(C67) = Uanis(C68) = Uanis(C69) =
Uanis(N20) = Uanis(C63) = Uanis(C62) = Uanis(C61) = Uanis(N19) = Uanis(C65) =
Uanis(C64)
Uanis(C78) = Uanis(C79) = Uanis(C80) = Uanis(N24) = Uanis(C76) = Uanis(C77) =
Uanis(C73) = Uanis(C72) = Uanis(C71) = Uanis(N22) = Uanis(C75) = Uanis(C74)
Uanis(N6) = Uanis(C20) = Uanis(C19) = Uanis(C18) = Uanis(C17) = Uanis(C16) =
Uanis(N5) = Uanis(C13) = Uanis(C12) = Uanis(C11) = Uanis(N4) = Uanis(C15) =
Uanis(C14)
Uanis(N7) = Uanis(C25) = Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24) =
Uanis(N8) = Uanis(C28) = Uanis(C29) = Uanis(C30) = Uanis(N9) = Uanis(C26) =
Uanis(C27)
Uanis(N1) = Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) =
Uanis(N2) = Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(N3) =
Uanis(C6)
Uanis(O16) = Uanis(O15) = Uanis(C111) = Uanis(C112) = Uanis(C113) = Uanis(C117)
= Uanis(C116) = Uanis(C114) = Uanis(C115) = Uanis(O14) = Uanis(O13)
Uanis(O12) = Uanis(C105) = Uanis(O11) = Uanis(C104) = Uanis(C106) = Uanis(C103)
= Uanis(C107) = Uanis(C102) = Uanis(C101) = Uanis(O10) = Uanis(O9)
Uanis(O1) = Uanis(O2) = Uanis(C81) = Uanis(C82) = Uanis(C83) = Uanis(C84) =
Uanis(C85) = Uanis(C86) = Uanis(C87) = Uanis(O4) = Uanis(O3)
Uanis(O20) = Uanis(C125) = Uanis(O19) = Uanis(C124) = Uanis(C123) = Uanis(C126)
= Uanis(C127) = Uanis(C122) = Uanis(C121) = Uanis(O18) = Uanis(O17)
Uanis(O23) = Uanis(C135) = Uanis(O24) = Uanis(C134) = Uanis(C136) = Uanis(C137)
= Uanis(C133) = Uanis(C132) = Uanis(C131)
Uanis(N16) = Uanis(C55) = Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54)
Uanis(C157) = Uanis(C152) = Uanis(C151) = Uanis(O29) = Uanis(O30) = Uanis(C153)
= Uanis(C154) = Uanis(C156) = Uanis(C155) = Uanis(O32) = Uanis(O31)
Uanis(O26) = Uanis(C145) = Uanis(O25) = Uanis(C144) = Uanis(C143) = Uanis(C146)
= Uanis(C142) = Uanis(C147) = Uanis(C141) = Uanis(O27) = Uanis(O28)
Uanis(C60) = Uanis(N18) = Uanis(C56) = Uanis(C57) = Uanis(C58) = Uanis(C59) =
Uanis(N17) = Uanis(C53) = Uanis(C55) = Uanis(C54) = Uanis(C52) = Uanis(C51) =
Uanis(N16)
Uanis(O5) = Uanis(C91) = Uanis(O6) = Uanis(C92) = Uanis(C97) = Uanis(C93) =
Uanis(C98) = Uanis(C96) = Uanis(C95) = Uanis(O8) = Uanis(O7)
Uanis(C93) = Uanis(C94) = Uanis(C95) = Uanis(O8) = Uanis(C91) = Uanis(C92) =
Uanis(C98) = Uanis(C96) = Uanis(C97) = Uanis(O6) = Uanis(O5) = Uanis(O7)
Uanis(O24) = Uanis(C135) = Uanis(O23) = Uanis(C134) = Uanis(C133) = Uanis(C136)
= Uanis(C137) = Uanis(C132) = Uanis(C131) = Uanis(O21) = Uanis(O22)
5. Others
 Fixed Sof: C97(0.5) H97A(0.5) H97B(0.5) H97C(0.5) C98(0.5) H98A(0.5)
 H98B(0.5) H98C(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C82(H82A,H82B), C86(H86A,H86B), C92(H92A,H92B), C94(H94A,H94B), C142(H14A,
 H14B), C144(H14C,H14D), C152(H15A,H15B), C154(H15C,H15D), C102(H10A,H10B),
 C104(H10C,H10D), C112(H11B,H11C), C114(H11D,H11E), C122(H12A,H12B), C124(H12C,
 H12D), C132(H13A,H13B), C134(H13C,H13D)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), N17(H17), N23(H23), C1(H1), C2(H2A), C4(H4), C5(H5A), C6(H6),
 C7(H7), C9(H9), C10(H10), C11(H11), C12(H12), C14(H14), C15(H15), C16(H16),
 C17(H17A), C19(H19), C20(H20), C51(H51), C52(H52), C54(H54), C55(H55),
 C56(H56), C57(H57), C59(H59), C60(H60), C71(H71), C72(H72), C74(H74), C75(H75),
  C76(H76), C77(H77), C79(H79), C80(H80), N8(H8), N11(H11A), N14(H14K),
 N20(H20A), C21(H21), C22(H22), C24(H24), C25(H25), C26(H26), C27(H27),
 C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37),
  C39(H39), C40(H40), C41(H41), C42(H42), C44(H44), C45(H45), C46(H46),
 C47(H47), C49(H49), C50(H50), C61(H61), C62(H62), C64(H64), C65(H65), C66(H66),
  C67(H67), C69(H69), C70(H70)
6.c Idealised Me refined as rotating group:
 C84(H84A,H84B,H84C), C85(H85A,H85B,H85C), C96(H96A,H96B,H96C), C97(H97A,H97B,
 H97C), C98(H98A,H98B,H98C), C146(H14E,H14F,H14G), C147(H14H,H14I,H14J),
 C156(H15E,H15F,H15G), C157(H15H,H15I,H15J), C106(H10E,H10F,H10G), C107(H10H,
 H10I,H10J), C116(H11F,H11G,H11H), C117(H11I,H11J,H11K), C126(H12E,H12F,H12G),
 C127(H12H,H12I,H12J), C136(H13E,H13F,H13G), C137(H13H,H13I,H13J)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'