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_4349559
_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         'C28 H32 Cu N12 O4, Cl'
_chemical_formula_sum            'C28 H32 Cl Cu N12 O4'
_chemical_formula_weight         699.64
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2014-10-25
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_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                   27.9361(13)
_cell_length_b                   25.4180(14)
_cell_length_c                   6.0524(3)
_cell_measurement_reflns_used    7143
_cell_measurement_temperature    293.15
_cell_measurement_theta_max      72.3260
_cell_measurement_theta_min      4.6850
_cell_volume                     4297.7(4)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      293.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega    1.00   75.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000   90.0000 74

  2 omega  -31.00   63.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -77.0000    0.0000 94

  3 omega   20.00  104.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -30.0000 84

  4 omega    1.00   75.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000    0.0000 74

  5 omega    1.00   75.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000  -60.0000 74

  6 omega   20.00  104.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  120.0000 84

  7 omega   39.00  109.00   1.0000   29.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  150.0000 70

  8 omega   87.00  178.00   1.0000   29.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000 -180.0000 91

  9 omega   39.00  109.00   1.0000   29.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -90.0000 70

 10 omega   38.00   91.00   1.0000   29.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -31.0000  -19.0000 53

 11 omega   39.00  109.00   1.0000   29.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   90.0000 70

 12 omega   81.00  176.00   1.0000   29.5750
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000   90.0000 95

 13 omega  -31.00   53.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000 -180.0000 84

 14 omega   10.00  104.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000   30.0000 94

 15 omega   10.00  104.00   1.0000    7.3950
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000 -150.0000 94
;
_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      -0.0181758000
_diffrn_orient_matrix_UB_12      0.0541797000
_diffrn_orient_matrix_UB_13      -0.0775409000
_diffrn_orient_matrix_UB_21      -0.0434253000
_diffrn_orient_matrix_UB_22      -0.0266162000
_diffrn_orient_matrix_UB_23      -0.1094857000
_diffrn_orient_matrix_UB_31      -0.0287546000
_diffrn_orient_matrix_UB_32      0.0059183000
_diffrn_orient_matrix_UB_33      0.2160405000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0284
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -4
_diffrn_reflns_number            21536
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         67.048
_diffrn_reflns_theta_min         4.704
_diffrn_source                   'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26924
_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    1.081
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.982
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         3922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1013
_refine_ls_R_factor_gt           0.0924
_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^)+(0.1410P)^2^+5.7200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2630
_refine_ls_wR_factor_ref         0.2698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3221
_reflns_number_total             3922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00386a2.cif
_cod_data_source_block           llclrr
_cod_database_code               4349559
_shelxl_version_number           2014-1
_reflns_odcompleteness_completeness 99.44
_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:
 C23(H23A,H23B), C17(H17A,H17B), C1(H1A,H1B), C63(H63A,H63B)
2.b Aromatic/amide H refined with riding coordinates:
 C46(H46), N4(H4), N15(H15), C34(H34), C50(H50), C58(H58), C81(H81), C3(H3)
;
_shelx_res_checksum              20896
_shelx_hkl_checksum              57379
_olex2_submission_special_instructions 'No special instructions were received'