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_7244270
_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         'C42 H42 Cu N10, 2(Cl O4), 0.33(O)'
_chemical_formula_sum            'C42 H42.67 Cl2 Cu N10 O8.33'
_chemical_formula_weight         955.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-27
_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                 94.546(2)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   17.0485(4)
_cell_length_b                   21.1841(6)
_cell_length_c                   17.4301(5)
_cell_measurement_reflns_used    5637
_cell_measurement_temperature    120.0(4)
_cell_measurement_theta_max      74.0580
_cell_measurement_theta_min      3.7850
_cell_volume                     6275.2(3)
_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      120.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3095
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_details
;
  1 omega  -59.00  -22.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000 -180.0000 37

  2 omega  -63.00   23.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000   30.0000 86

  3 omega  -55.00   39.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   19.0000  -60.0000 94

  4 omega   30.00   57.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       41.9589   57.0000  150.0000 27

  5 omega   34.00  146.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6025  -15.0000  -30.0000 112

  6 omega   62.00  128.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6025  -45.0000   30.0000 66

  7 omega   65.00   92.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6025  -49.0000 -162.0000 27

  8 omega   32.00  127.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6025  -30.0000  150.0000 95

  9 omega   85.00  127.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6025  -61.0000  -30.0000 42

 10 omega   85.00  178.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      105.6025   30.0000  -30.0000 93
;
_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      -0.0668116000
_diffrn_orient_matrix_UB_12      0.0009523000
_diffrn_orient_matrix_UB_13      0.0545559000
_diffrn_orient_matrix_UB_21      -0.0490896000
_diffrn_orient_matrix_UB_22      -0.0442645000
_diffrn_orient_matrix_UB_23      -0.0550393000
_diffrn_orient_matrix_UB_31      0.0365458000
_diffrn_orient_matrix_UB_32      -0.0576518000
_diffrn_orient_matrix_UB_33      0.0432464000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0861
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            25753
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.268
_diffrn_reflns_theta_min         3.290
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.488
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.839
_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    1.517
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2966
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.369
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.47(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1724
_refine_ls_number_reflns         17802
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0615
_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^)+(0.0644P)^2^+4.4032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1443
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.945
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                13561
_reflns_number_total             17802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra07811a2.cif
_cod_data_source_block           cu-h
_cod_database_code               7244270
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C252 H256 Cl12 Cu6 N60 O50'
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.771
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.53(2)
 0.47(2)
2. 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
3.a Aromatic/amide H refined with riding coordinates:
 N13(H13), N15(H15), N18(H18), N20(H20), C44(H44), C45(H45), C46(H46),
 C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C59(H59), C60(H60), C61(H61),
  C62(H62), C63(H63), C65(H65), C66(H66), C67(H67), C72(H72), C73(H73),
 C74(H74), C75(H75), C76(H76), C80(H80), C81(H81), C82(H82), C83(H83), C84(H84),
  N23(H23), N25(H25), N28(H28), N30(H30), C86(H86), C87(H87), C88(H88),
 C93(H93), C94(H94), C95(H95), C96(H96), C97(H97), C101(H101), C102(H102),
 C103(H103), C104(H104), C105(H105), C107(H107), C108(H108), C109(H109),
 C114(H114), C115(H115), C116(H116), C117(H117), C118(H118), C122(H122),
 C123(H123), C124(H124), C125(H125), C126(H126), C2(H2), N3(H3), C3(H3A),
 C4(H4), N5(H5), N8(H8), C9(H9), N10(H10), C10(H10A), C11(H11), C12(H12),
 C13(H13A), C17(H17), C18(H18A), C19(H19), C20(H20A), C21(H21), C23(H23A),
 C24(H24), C25(H25A), C30(H30A), C31(H31), C32(H32), C33(H33), C34(H34),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
3.b Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C57(H57A,H57B,H57C), C70(H70A,H70B,H70C), C78(H78A,H78B,
 H78C), C91(H91A,H91B,H91C), C99(H99A,H99B,H99C), C112(H11A,H11B,H11C),
 C120(H12A,H12B,H12C), C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C28(H28A,H28B,
 H28C), C36(H36A,H36B,H36C)
;
_olex2_submission_special_instructions 'No special instructions were received'