Simple One-Pot Preparation of a Rapid Response AIE Fluorescent Metal-Organic Framework.
Rouhani, Farzaneh; Morsali, Ali; Retailleau, Pascal; ACS applied materials & interfaces 10 (2018) 36259–36266; doi:10.1021/acsami.8b12404

data_4515323
_publ_section_title
;
 Simple One-Pot Preparation of a Rapid Response AIE Fluorescent
 Metal-Organic Framework.
;
_journal_issue                   42
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              36259
_journal_page_last               36266
_journal_paper_doi               10.1021/acsami.8b12404
_journal_volume                  10
_journal_year                    2018
_chemical_formula_moiety         'C22 H18 Co N4 O4, C3 H7 N O'
_chemical_formula_sum            'C25 H25 Co N5 O5'
_chemical_formula_weight         534.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                90
_cell_angle_beta                 92.308(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9663(5)
_cell_length_b                   16.9221(10)
_cell_length_c                   15.1938(8)
_cell_measurement_reflns_used    7181
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.1110
_cell_measurement_theta_min      4.0870
_cell_volume                     2560.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7b (Rigaku OD, 2015)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     63.00  89.00   0.50   12.00    --   -0.30  57.00 -90.00   52
  2  \w    -26.00  59.00   0.50   12.00    --   -0.30  57.00  90.00  170
  3  \w    -10.00  42.00   0.50   12.00    --   -0.30  57.00 -30.00  104
  4  \w    -25.00  88.00   0.50   12.00    --   -0.30  57.00 150.00  226
  5  \w     -8.00  18.00   0.50   12.00    --   -0.30  38.00 150.00   52
  6  \w     51.00  83.00   0.50   12.00    --   -0.30  57.00-180.00   64
  7  \w    -12.00  14.00   0.50   12.00    --   -0.30  57.00-150.00   52
  8  \w     16.00  47.00   0.50   12.00    --   -0.30  57.00 -90.00   62
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Pro: Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0261467000
_diffrn_orient_matrix_UB_12      -0.0388338000
_diffrn_orient_matrix_UB_13      -0.0044520000
_diffrn_orient_matrix_UB_21      0.0580331000
_diffrn_orient_matrix_UB_22      -0.0151807000
_diffrn_orient_matrix_UB_23      0.0226968000
_diffrn_orient_matrix_UB_31      -0.0320161000
_diffrn_orient_matrix_UB_32      0.0042322000
_diffrn_orient_matrix_UB_33      0.0405857000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43694
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         30.746
_diffrn_reflns_theta_min         3.521
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Rigaku mm03 '
_exptl_absorpt_coefficient_mu    0.715
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       cobblestone
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     333
_refine_ls_number_reflns         7255
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0515
_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^)+(0.0840P)^2^+0.8931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1598
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4923
_reflns_number_total             7255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b12404_si_003.cif
_cod_data_source_block           TMU-40(Co)
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '__diffrn_measurement_device' was replaced with
'_diffrn_measurement_device'.

Automatic conversion script
Id: cif_correct_tags 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4515323
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N2-H2 = N3-H3
 0.87 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C12(H12), C13(H13),
 C19(H19), C20(H20), C21(H21), C22(H22), C102(H102)
3.c Idealised Me refined as rotating group:
 C104(H10A,H10B,H10C), C105(H10D,H10E,H10F)
;
_shelx_res_checksum              23533
_shelx_hkl_checksum              80176