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_1560784
_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         'C34 H38 N6 O8 Zn2'
_chemical_formula_sum            'C34 H38 N6 O8 Zn2'
_chemical_formula_weight         789.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 110.340(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   47.393(4)
_cell_length_b                   8.9045(8)
_cell_length_c                   17.3687(15)
_cell_measurement_reflns_used    6112
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.373
_cell_measurement_theta_min      2.333
_cell_volume                     6872.7(10)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0488
_diffrn_reflns_av_unetI/netI     0.0577
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -57
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12231
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.83
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.78
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0823 before and 0.0572 after correction.
 The Ratio of minimum to maximum transmission is 0.78.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0970 before and 0.0695 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 70553 reflections, Rint = 0.0742
 (19339 with I > 3sig(I), Rint = 0.0523)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.492
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         6352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+5.1581P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0969
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                4733
_reflns_number_total             6352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            0zn33dmgdpadisorderfinal.cif
_cod_data_source_block           c2c
_cod_original_cell_volume        6872.7(11)
_cod_database_code               1560784
_olex2_refinement_description
;
1. 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
2. Others
 Fixed Sof: O7(0.5) O7A(0.5) O8(0.5) O8A(0.5) C16(0.5) H16(0.5) C16A(0.5)
 H16A(0.5) C17(0.5) H17(0.5) C17A(0.5) H17A(0.5) C19(0.5) H19(0.5) C19A(0.5)
 H19A(0.5) C20(0.5) H20(0.5) C20A(0.5) H20A(0.5) C31(0.5) H31C(0.5) H31D(0.5)
 C31A(0.5) H31A(0.5) H31B(0.5) C32(0.5) C32A(0.5) C33(0.5) H33D(0.5) H33E(0.5)
 H33F(0.5) C33A(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5) H34D(0.5) H34E(0.5)
 H34F(0.5) C34A(0.5) H34A(0.5) H34B(0.5) H34C(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C24(H24A,H24B), C29(H29A,H29B), C31(H31C,H31D), C31A(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), 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), C16A(H16A),
 C17(H17), C17A(H17A), C19(H19), C19A(H19A), C20(H20), C20A(H20A)
3.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C33(H33D,H33E,H33F), C33A(H33A,H33B,
 H33C), C34(H34D,H34E,H34F), C34A(H34A,H34B,H34C)
;
_olex2_submission_special_instructions 'No special instructions were received'