A long-range emissive mega-Stokes inorganic–organic hybrid material with peripheral carboxyl functionality for As(v) recognition and its application in bioimaging
Venkateswarulu, M.; Gambhir, Diksha; Kaur, Harpreet; Daniel, P. Vineeth; Mondal, Prosenjit; Koner, Rik Rani; Dalton Trans.  (2017) –; doi:10.1039/C7DT02387A

data_7044322
_publ_section_title
;
 A long-range emissive mega-Stokes inorganic--organic hybrid material with
 peripheral carboxyl functionality for As(v) recognition and its
 application in bioimaging
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02387A
_journal_year                    2017
_chemical_formula_moiety         'C16 H18 Cu N4 O4, 3(H2 O), C2 H6 O'
_chemical_formula_sum            'C18 H30 Cu N4 O8'
_chemical_formula_weight         494.00
_chemical_name_systematic        PTCA-Cu
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-06-28
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2017-06-28 deposited with the CCDC.
2017-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 97.823(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5798(2)
_cell_length_b                   11.2874(3)
_cell_length_c                   22.5286(5)
_cell_measurement_reflns_used    4981
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      66.8080
_cell_measurement_theta_min      4.3840
_cell_volume                     2161.45(9)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43i (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9987
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -8.00  91.00   1.00    1.50    --   25.57  57.00 -30.00   99
  2  \w    113.00 144.00   1.00    5.00    --   66.78 111.00-120.00   31
  3  \w     99.00 178.00   1.00   10.00    --  108.00 138.00 -60.00   79
  4  \w    153.00 178.00   1.00   10.00    --  108.00 104.00 -30.00   25
  5  \w    102.00 141.00   1.00   10.00    --  108.00 104.00 -30.00   39
  6  \w     86.00 147.00   1.00    5.00    --   66.78 164.00 -76.00   61
  7  \w     61.00 131.00   1.00    5.00    --   66.78 178.00  90.00   70
  8  \w     63.00 162.00   1.00   10.00    --  108.00  43.00 120.00   99
  9  \w     72.00 167.00   1.00   10.00    --  108.00  21.00  90.00   95
 10  \w    102.00 144.00   1.00   10.00    --  108.00 -89.00-120.00   42
 11  \w     71.00 157.00   1.00   10.00    --  108.00 -89.00-150.00   86
 12  \w     62.00 112.00   1.00   10.00    --  108.00-104.00  30.00   50
 13  \w     30.00  68.00   1.00   10.00    --  108.00  21.00  90.00   38
 14  \w     31.00 136.00   1.00    5.00    --   66.78  63.00 -30.00  105
 15  \w     32.00  57.00   1.00   10.00    --  108.00 -89.00-150.00   25
 16  \w     22.00  79.00   1.00   10.00    --  108.00 -89.00-120.00   57
 17  \w     -7.00  90.00   1.00    5.00    --   66.78 -38.00-180.00   97
 18  \w    -10.00  82.00   1.00    1.50    --   25.57  57.00-180.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0132477000
_diffrn_orient_matrix_UB_12      -0.0036125000
_diffrn_orient_matrix_UB_13      -0.0674584000
_diffrn_orient_matrix_UB_21      0.0278769000
_diffrn_orient_matrix_UB_22      0.1348560000
_diffrn_orient_matrix_UB_23      0.0004468000
_diffrn_orient_matrix_UB_31      0.1786395000
_diffrn_orient_matrix_UB_32      -0.0208720000
_diffrn_orient_matrix_UB_33      0.0145123000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0149
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            7105
_diffrn_reflns_theta_full        66.79
_diffrn_reflns_theta_max         66.79
_diffrn_reflns_theta_min         4.39
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.894
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43i (Rigaku Oxford Diffraction, 2015)
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    1.518
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.123
_exptl_crystal_size_mid          0.107
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.029
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         3781
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0545P)^2^+4.0830P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                3565
_reflns_number_total             3781
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt02387a2.cif
_cod_data_source_block           mof_17_lt_cu
_cod_original_cell_volume        2161.44(9)
_cod_database_code               7044322
_chemical_oxdiff_formula         'C72 H120 Cu4 N16 O32'
_reflns_odcompleteness_completeness 97.96
_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,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All N(H) groups, All O(H,H) groups
2. Restrained distances
 N4-H4A
 0.85 with sigma of 0.01
 N3-H3A
 0.85 with sigma of 0.01
 C4-H4A
 1.893758 with sigma of 0.02
 C3-H3A
 1.914016 with sigma of 0.02
3.a Free rotating group:
 O1(H1E,H1F), O6(H6A,H6B), O7(H7A,H7B)
3.b Rotating group:
 O8(H8)
3.c Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), N1(H1A,H1B), C2(H2C,H2D), C1(H1C,H1D), C18(H18A,H18B)
3.d Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C15(H15), C16(H16), C3(H3), C4(H4)
3.e Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C)
;
_olex2_date_sample_data_collection 2014-06-26
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.438
_oxdiff_exptl_absorpt_empirical_full_min 0.779