[9]aneN<sub>3</sub>-based fluorescent receptors for metal ion sensing, featuring urea and amide functional groups.
Garau, Alessandra; Bencini, Andrea; Blake, Alexander J.; Caltagirone, Claudia; Conti, Luca; Isaia, Francesco; Lippolis, Vito; Montis, Riccardo; Mariani, Palma; Scorciapino, Mariano Andrea; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4949–4960; doi:10.1039/c9dt00288j

data_7049372
_publ_section_title
;
 [9]aneN<sub>3</sub>-based fluorescent receptors for metal ion sensing,
 featuring urea and amide functional groups.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4949
_journal_page_last               4960
_journal_paper_doi               10.1039/c9dt00288j
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C39 H38 Cu N9 O3, N O3'
_chemical_formula_sum            'C39 H38 Cu N10 O6'
_chemical_formula_weight         806.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-27
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2019-01-08 deposited with the CCDC.    2019-03-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8909(3)
_cell_length_b                   10.8298(3)
_cell_length_c                   39.2281(14)
_cell_measurement_reflns_used    10457
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      72.3150
_cell_measurement_theta_min      4.9620
_cell_volume                     7175.8(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(12)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2349
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega -109.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000   90.0000 77

  2 omega  -50.00   15.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 65

  3 omega  -36.00   31.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000 -150.0000 67

  4 omega  -26.00   10.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       42.8292  -57.0000    0.0000 36

  5 omega   34.00   61.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000   90.0000 27

  6 omega   35.00   87.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000   30.0000 52

  7 omega  142.00  169.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000 -180.0000 27

  8 omega   91.00  123.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000 -180.0000 32

  9 omega   43.00  112.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -61.0000   90.0000 69

 10 omega   40.00   86.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -120.0000 46

 11 omega   80.00  175.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000 -150.0000 95

 12 omega   28.00  149.00   1.0000   80.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -15.0000 -150.0000 121
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'GV1000, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0632118000
_diffrn_orient_matrix_UB_12      0.0924950000
_diffrn_orient_matrix_UB_13      -0.0121076000
_diffrn_orient_matrix_UB_21      0.0011680000
_diffrn_orient_matrix_UB_22      -0.0624875000
_diffrn_orient_matrix_UB_23      -0.0352831000
_diffrn_orient_matrix_UB_31      -0.0658021000
_diffrn_orient_matrix_UB_32      0.0880556000
_diffrn_orient_matrix_UB_33      -0.0122847000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            30968
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.734
_diffrn_reflns_theta_min         4.980
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'GV1000 (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.400
_exptl_absorpt_correction_T_max  0.896
_exptl_absorpt_correction_T_min  0.786
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
            a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_description       lath
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         7048
_refine_ls_number_restraints     507
_refine_ls_restrained_S_all      1.154
_refine_ls_R_factor_all          0.1031
_refine_ls_R_factor_gt           0.0981
_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^)+80.3000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2177
_refine_ls_wR_factor_ref         0.2196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6390
_reflns_number_total             7048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00288j2.cif
_cod_data_source_block           vlajbi
_cod_depositor_comments
'Adding full bibliography for 7049370--7049372.cif.'
_cod_original_cell_volume        7175.8(4)
_cod_database_code               7049372
_chemical_oxdiff_formula         'C39 H38 N10 O6 Cu'
_chemical_oxdiff_usercomment
'GVB-711 #15085 VLAJBI mounted in fomblin on micromount'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C19(H19A,H19B), C14(H14A,H14B), C18(H18A,H18B), C30(H30A,
 H30B), C13(H13A,H13B), C16(H16A,H16B), C12(H12A,H12B), C11(H11A,H11B)
3.b Aromatic/amide H refined with riding coordinates:
 N5(H5), N8(H8), C40(H40), C34(H34), C33(H33), C35(H35), C20(H20), C38(H38),
 C39(H39), C21(H21), C28(H28), C26(H26), C27(H27), C22(H22), C9(H9), C8(H8A),
 C7(H7), C1(H1), C2(H2), C3(H3)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'