Multipurpose made colorimetric materials for amines, pH change and metal ion detection
Bao, Lihong; Jones, Leighton O.; Garrote Cañas, Ana M.; Yan, Yunhan; Pask, Christopher M.; Hardie, Michaele J.; Mosquera, Martin A.; Schatz, George C.; Sergeeva, Natalia N.; RSC Advances 12 (2022) 2684–2692; doi:10.1039/D1RA07811A

data_7244267
_publ_section_title
;
 Multipurpose made colorimetric materials for amines, pH change and metal
 ion detection
;
_journal_issue                   5
_journal_name_full               'RSC Advances'
_journal_page_first              2684
_journal_page_last               2692
_journal_paper_doi               10.1039/D1RA07811A
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C23 H26 N5 O2, Cl O4'
_chemical_formula_sum            'C23 H26 Cl N5 O6'
_chemical_formula_weight         503.94
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-05-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-05-27 deposited with the CCDC.	2022-01-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.6704(6)
_cell_length_b                   17.4161(8)
_cell_length_c                   19.5839(10)
_cell_measurement_reflns_used    1134
_cell_measurement_temperature    120.00(14)
_cell_measurement_theta_max      71.9030
_cell_measurement_theta_min      4.6670
_cell_volume                     4662.6(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
  1 omega  -45.00  -19.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000  150.0000 26

  2 omega  -47.00   27.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000   30.0000 74

  3 omega  -14.00   19.00   1.0000    7.5000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000  150.0000 33

  4 omega   91.00  128.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -61.0000 -150.0000 37

  5 omega   45.00   89.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -61.0000 -150.0000 44

  6 omega   41.00  142.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -15.0000  -90.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0985036000
_diffrn_orient_matrix_UB_12      0.0307703000
_diffrn_orient_matrix_UB_13      0.0267146000
_diffrn_orient_matrix_UB_21      -0.0270759000
_diffrn_orient_matrix_UB_22      0.0809737000
_diffrn_orient_matrix_UB_23      -0.0252688000
_diffrn_orient_matrix_UB_31      -0.0475623000
_diffrn_orient_matrix_UB_32      0.0176864000
_diffrn_orient_matrix_UB_33      0.0696104000
_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     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            2767
_diffrn_reflns_point_group_measured_fraction_full 0.677
_diffrn_reflns_point_group_measured_fraction_max 0.655
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.458
_diffrn_reflns_theta_min         4.691
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.890
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.53434
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details
;
 Flack x determined using 297 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         1544
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0930P)^2^+5.4340P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.297
_reflns_Friedel_fraction_full    0.334
_reflns_Friedel_fraction_max     0.310
_reflns_number_gt                1433
_reflns_number_total             1544
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra07811a2.cif
_cod_data_source_block           yy10_cu
_cod_database_code               7244267
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C184 H208 Cl8 N40 O48'
_reflns_odcompleteness_completeness 93.60
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Cl1-O2 = Cl1-O3 = Cl1-O5 = Cl1-O4
 1.44 with sigma of 0.01
 Cl1-O2 \\sim Cl1-O3 \\sim Cl1-O4 \\sim Cl1-O5
 with sigma of 0.01
3. Others
 Fixed Sof: O3(0.6) O4(0.4) O5(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), N3(H3), C3(H3A), C7(H7), C8(H8), C10(H10), C11(H11)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C12(H12A,H12B,H12C)
;
_olex2_date_sample_data_collection 2016-04-12
_olex2_submission_special_instructions 'No special instructions were received'