The dicyclen‒TPE zinc complex as a novel fluorescent ensemble for nanomolar pyrophosphate sensing in 100% aqueous solution
Xu, Hao-Ran; Li, Kun; Wang, Ming-Qi; Wang, Bo-Lin; Wang, Xin; Yu, Xiao-Qi; Org. Chem. Front. 1 (2014) 1276–; doi:10.1039/C4QO00243A

data_1553039
_publ_section_title
;
 The dicyclen--TPE zinc complex as a novel fluorescent ensemble for
 nanomolar pyrophosphate sensing in 100% aqueous solution
;
_journal_issue                   11
_journal_name_full               'Org. Chem. Front.'
_journal_page_first              1276
_journal_paper_doi               10.1039/C4QO00243A
_journal_volume                  1
_journal_year                    2014
_chemical_formula_moiety         'C44 H54 Cl2 N8 Zn2, 2(N O3)'
_chemical_formula_sum            'C44 H54 Cl2 N10 O6 Zn2'
_chemical_formula_weight         1020.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                96.785(7)
_cell_angle_beta                 111.858(7)
_cell_angle_gamma                102.580(7)
_cell_formula_units_Z            2
_cell_length_a                   13.7485(11)
_cell_length_b                   14.2439(12)
_cell_length_c                   16.1369(12)
_cell_measurement_reflns_used    5617
_cell_measurement_temperature    145.2(3)
_cell_measurement_theta_max      27.9400
_cell_measurement_theta_min      3.2540
_cell_volume                     2792.4(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-2012 (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      145.2(3)
_diffrn_detector_area_resol_mean 16.0874
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0394815000
_diffrn_orient_matrix_UB_12      0.0257929000
_diffrn_orient_matrix_UB_13      -0.0165637000
_diffrn_orient_matrix_UB_21      0.0275301000
_diffrn_orient_matrix_UB_22      0.0207295000
_diffrn_orient_matrix_UB_23      -0.0258852000
_diffrn_orient_matrix_UB_31      -0.0323182000
_diffrn_orient_matrix_UB_32      -0.0405040000
_diffrn_orient_matrix_UB_33      -0.0375846000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.1103
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23678
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.862
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.003
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.929
_refine_diff_density_min         -1.537
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         11355
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1470
_refine_ls_R_factor_gt           0.1131
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.2000P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3085
_refine_ls_wR_factor_ref         0.3414
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6807
_reflns_number_total             11355
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4qo00243a2.cif
_cod_data_source_block           140120_s3_xhr
_cod_database_code               1553039
_shelxl_version_number           2013-2
_chemical_oxdiff_formula         c12h12n2o3zn2p2
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.720
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N9-O3
 1.32 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Uanis(N9) = Uanis(N10)
Uanis(O1) = Uanis(O2) = Uanis(O3) = Uanis(O4) = Uanis(O5) = Uanis(O6)
4.a Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B),
 C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B),
  C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23),
  C25(H25), C26(H26)
;
_shelx_res_checksum              58338
_shelx_hkl_checksum              80596