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_7244272
_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 N10 Zn, 2(Cl O4), 0.33(H2 O)'
_chemical_formula_sum            'C42 H42.67 Cl2 N10 O8.33 Zn'
_chemical_formula_weight         957.13
_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   mixed
_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                 94.0351(15)
_cell_angle_gamma                90
_cell_formula_units_Z            6
_cell_length_a                   17.0846(3)
_cell_length_b                   21.1938(4)
_cell_length_c                   17.4229(3)
_cell_measurement_reflns_used    12705
_cell_measurement_temperature    120.1(3)
_cell_measurement_theta_max      73.5280
_cell_measurement_theta_min      3.3250
_cell_volume                     6293.0(2)
_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      120.1(3)
_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 0.970
_diffrn_measurement_details
;
  1 omega  -62.00   30.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   57.0000   30.0000 92

  2 omega  -55.00  -29.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000 -180.0000 26

  3 omega  -25.00    8.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       42.7089  -57.0000 -180.0000 33

  4 omega   55.00  124.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -30.0000  -90.0000 69

  5 omega   78.00  120.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -64.0000  -64.6604 42

  6 omega   70.00   99.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -45.0000 -180.0000 29

  7 omega   37.00   93.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -62.0000  -84.7241 56

  8 omega   84.00  119.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775   61.0000   60.0000 35

  9 omega   37.00  131.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -61.0000  120.0000 94

 10 omega   26.00  132.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9775  -15.0000  120.0000 106

 11 omega -107.00  -17.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -57.0000 -120.0000 90
;
_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      0.0096961000
_diffrn_orient_matrix_UB_12      0.0657480000
_diffrn_orient_matrix_UB_13      0.0371281000
_diffrn_orient_matrix_UB_21      -0.0717514000
_diffrn_orient_matrix_UB_22      -0.0124452000
_diffrn_orient_matrix_UB_23      0.0466817000
_diffrn_orient_matrix_UB_31      0.0540965000
_diffrn_orient_matrix_UB_32      -0.0283546000
_diffrn_orient_matrix_UB_33      0.0656090000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            27217
_diffrn_reflns_point_group_measured_fraction_full 0.751
_diffrn_reflns_point_group_measured_fraction_max 0.713
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.943
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.771
_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    1.515
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2972
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.180
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 4444 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1744
_refine_ls_number_reflns         18199
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0492P)^2^+3.6677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.429
_reflns_Friedel_fraction_full    0.489
_reflns_Friedel_fraction_max     0.440
_reflns_number_gt                16494
_reflns_number_total             18199
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra07811a2.cif
_cod_data_source_block           zn-h
_cod_original_cell_volume        6292.97(18)
_cod_database_code               7244272
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C252 H256 Cl12 N60 O50 Zn6'
_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 N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Cl6-O23 = Cl6-O24 = Cl6-O25 = Cl6-O26
 1.43 with sigma of 0.005
3. Rigid body (RIGU) restrains
 O21, O22, O23, O24, O25, O26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O23(0.5) O24(0.5) O25(0.5) O26(0.5)
5.a Free rotating group:
 O27(H27A,H27B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), N3(H3), C3(H3A), C4(H4), N5(H5), N8(H8), C9(H9), N10(H10), C10(H10A),
 C11(H11), C12(H12), C13(H13), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C23(H23), C24(H24), C25(H25), C30(H30), C31(H31), C32(H32), C33(H33),
 C34(H34), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), N23(H23A),
 N25(H25A), N28(H28), N30(H30A), 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), N13(H13A), N15(H15), N18(H18A), N20(H20A),
 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)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C36(H36A,H36B,
 H36C), C91(H91A,H91B,H91C), C99(H99A,H99B,H99C), C112(H11A,H11B,H11C),
 C119(H11D,H11E,H11F), C49(H49A,H49B,H49C), C57(H57A,H57B,H57C), C70(H70A,H70B,
 H70C), C78(H78A,H78B,H78C)
;
_olex2_submission_special_instructions 'No special instructions were received'