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_7244268
_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         'C46 H50 Cu N10 O4, 2(Cl O4)'
_chemical_formula_sum            'C46 H50 Cl2 Cu N10 O12'
_chemical_formula_weight         1069.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_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                   13.6541(5)
_cell_length_b                   20.9932(10)
_cell_length_c                   33.7804(15)
_cell_measurement_reflns_used    2743
_cell_measurement_temperature    120.01(19)
_cell_measurement_theta_max      72.7590
_cell_measurement_theta_min      4.9570
_cell_volume                     9682.9(7)
_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      120.01(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
  1 omega -104.00   35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000    0.0000  -30.0000 139

  2 omega   87.00  173.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775   45.0000  120.0000 86

  3 omega  112.00  164.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775   61.0000    0.0000 52

  4 omega   98.00  172.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775   61.0000 -120.0000 74

  5 omega  100.00  127.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -45.0000 -180.0000 27

  6 omega   39.00   67.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -45.0000 -180.0000 28
;
_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      0.1032066000
_diffrn_orient_matrix_UB_12      -0.0298905000
_diffrn_orient_matrix_UB_13      -0.0001072000
_diffrn_orient_matrix_UB_21      -0.0282406000
_diffrn_orient_matrix_UB_22      -0.0409021500
_diffrn_orient_matrix_UB_23      -0.0360885500
_diffrn_orient_matrix_UB_31      0.0362397000
_diffrn_orient_matrix_UB_32      0.0530753000
_diffrn_orient_matrix_UB_33      -0.0278114000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            5787
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.310
_diffrn_reflns_theta_min         4.078
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.272
_exptl_absorpt_correction_T_max  0.590
_exptl_absorpt_correction_T_min  0.208
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       plate
_exptl_crystal_F_000             4440
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.909
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     170
_refine_ls_number_reflns         2365
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0675
_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^)+(0.0962P)^2^+61.9396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1857
_refine_ls_wR_factor_ref         0.1934
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2032
_reflns_number_total             2365
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra07811a2.cif
_cod_data_source_block           agc29
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7244268
_chemical_oxdiff_formula         'C368 H400 Cl16 Cu8 N80 O112'
_reflns_odcompleteness_completeness 99.03
_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. Rigid body (RIGU) restrains
 Cl1, O2, O2, O3, O3, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O3(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 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)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-06-15
_olex2_submission_special_instructions 'No special instructions were received'