Bromide anion-triggered visible responsive metallogels based on squaramide complexes
Wu, Di; Jiang, Ruyong; Luo, Liang; He, Zhen; You, Jingsong; Inorganic Chemistry Frontiers 3 (2016) 1597–; doi:10.1039/C6QI00386A

data_4349558
_publ_section_title
;
 Bromide anion-triggered visible responsive metallogels based on
 squaramide complexes
;
_journal_issue                   12
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1597
_journal_paper_doi               10.1039/C6QI00386A
_journal_volume                  3
_journal_year                    2016
_chemical_formula_moiety         'Br, C28 H32 Cu N12 O4'
_chemical_formula_sum            'C28 H32 Br Cu N12 O4'
_chemical_formula_weight         744.10
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2n 2ac'
_space_group_name_H-M_alt        'P c m n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-06-17
_audit_creation_method
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Olex2 1.2
(compiled 2014.05.21 svn.r2940 for OlexSys, GUI svn.r4846)
;
_audit_update_record
;
2015-05-21 deposited with the CCDC.
2016-10-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.06932(11)
_cell_length_b                   25.5373(6)
_cell_length_c                   27.9983(6)
_cell_measurement_reflns_used    11265
_cell_measurement_temperature    292.2(6)
_cell_measurement_theta_max      72.6310
_cell_measurement_theta_min      4.6360
_cell_volume                     4339.57(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution
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Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.2(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -31.00   53.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000  150.0000 84

  2 omega   10.00  104.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000   30.0000 94

  3 omega    1.00   75.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000    0.0000 74

  4 omega   10.00  104.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000    0.0000 94

  5 omega   20.00  104.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  120.0000 84

  6 omega   20.00  104.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -30.0000 84

  7 omega   91.00  176.00   1.0000   19.5900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -150.0000 85

  8 omega   39.00  109.00   1.0000   19.5900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 70

  9 omega   40.00   98.00   1.0000   19.5900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -30.0000 58

 10 omega   90.00  175.00   1.0000   19.5900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000 -180.0000 85

 11 omega   39.00  109.00   1.0000   19.5900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

 12 omega   38.00   91.00   1.0000   19.5900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

 13 omega   70.00  178.00   1.0000   19.5900
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  150.0000 108

 14 omega   40.00   98.00   1.0000   19.5900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000 -120.0000 58

 15 omega   10.00  104.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000 -150.0000 94

 16 omega   18.00  106.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   38.0000 -150.0000 88

 17 omega  -31.00   53.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000   60.0000 84

 18 omega   20.00  104.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -60.0000 84

 19 omega    1.00   75.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000 -180.0000 74

 20 omega  -31.00   53.00   1.0000    4.8950
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000 -120.0000 84

 21 omega   37.00  146.00   1.0000   19.5900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -15.0000   60.0000 109

 22 omega   40.00  116.00   1.0000   19.5900
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000   90.0000 76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0231665000
_diffrn_orient_matrix_UB_12      0.0444830000
_diffrn_orient_matrix_UB_13      0.0368454000
_diffrn_orient_matrix_UB_21      -0.1081890000
_diffrn_orient_matrix_UB_22      -0.0348881000
_diffrn_orient_matrix_UB_23      0.0382504000
_diffrn_orient_matrix_UB_31      0.2284561000
_diffrn_orient_matrix_UB_32      -0.0210325000
_diffrn_orient_matrix_UB_33      0.0143989000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            34401
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.073
_diffrn_reflns_theta_min         4.687
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.129
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60512
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.636
_refine_diff_density_min         -1.804
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3967
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.1054
_refine_ls_R_factor_gt           0.0980
_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^)+(0.1655P)^2^+16.2752P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3076
_refine_ls_wR_factor_ref         0.3134
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3374
_reflns_number_total             3967
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00386a2.cif
_cod_data_source_block           llbr
_cod_database_code               4349558
_shelxl_version_number           2014-1
_reflns_odcompleteness_completeness 99.84
_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 C(H,H) groups, All N(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C19(H19A,H19B), C32(H32A,H32B), C90(H90A,H90B)
2.b Aromatic/amide H refined with riding coordinates:
 N9(H9), N11(H11), N10(H10), C68(H68), C85(H85), C93(H93), C91(H91), C92(H92)
;
_shelx_res_checksum              96917
_shelx_hkl_checksum              80362
_olex2_submission_special_instructions 'No special instructions were received'