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_7244273
_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 H38 F12 N10 O4 Zn, 2(Cl O4)'
_chemical_formula_sum            'C46 H38 Cl2 F12 N10 O12 Zn'
_chemical_formula_weight         1287.13
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_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                 109.320(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1544(4)
_cell_length_b                   21.5464(4)
_cell_length_c                   18.6498(6)
_cell_measurement_reflns_used    14852
_cell_measurement_temperature    120.1(4)
_cell_measurement_theta_max      30.8300
_cell_measurement_theta_min      3.6170
_cell_volume                     4988.2(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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.1(4)
_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 0.908
_diffrn_measurement_details
;
  1 omega  -55.00   38.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -57.0000 -120.0000 93

  2 omega  -36.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509    0.0000   90.0000 134

  3 omega   54.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509    0.0000   90.0000 44

  4 omega  -37.00  -10.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509    0.0000   90.0000 27

  5 omega  -84.00    7.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322  -37.0000  -30.0000 91

  6 omega  -38.00   50.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -13.7322   57.0000  150.0000 88

  7 omega  -54.00  -27.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       12.9509  -37.0000 -120.0000 27
;
_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      -0.0271983000
_diffrn_orient_matrix_UB_12      0.0230884000
_diffrn_orient_matrix_UB_13      -0.0265105000
_diffrn_orient_matrix_UB_21      0.0486940000
_diffrn_orient_matrix_UB_22      0.0170197000
_diffrn_orient_matrix_UB_23      0.0082793000
_diffrn_orient_matrix_UB_31      0.0124260000
_diffrn_orient_matrix_UB_32      -0.0161517000
_diffrn_orient_matrix_UB_33      -0.0291996000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38078
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         31.243
_diffrn_reflns_theta_min         3.277
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.881
_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    1.714
_exptl_crystal_description       prism
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.492(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     753
_refine_ls_number_reflns         12468
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0364P)^2^+4.0692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0833
_refine_ls_wR_factor_ref         0.0872
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.908
_reflns_number_gt                11268
_reflns_number_total             12468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra07811a2.cif
_cod_data_source_block           zn-ocf3
_cod_database_code               7244273
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C184 H152 Cl8 F48 N40 O48 Zn4'
_shelx_estimated_absorpt_t_max   0.938
_shelx_estimated_absorpt_t_min   0.846
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.508(9)
 0.492(9)
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:
 C2(H2), N3(H3), C3(H3A), C4(H4), N5(H5), N8(H8), C9(H9), N10(H10), C10(H10A),
 C12(H12), C13(H13), C18(H18), C19(H19), C21(H21), C22(H22), C25(H25), C26(H26),
  C27(H27), C32(H32), C33(H33), C35(H35), C36(H36), C41(H41), C42(H42),
 C44(H44), C45(H45)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C16(H16A,H16B,H16C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C)
;
_olex2_submission_special_instructions 'No special instructions were received'