Fluorescent phenoxy benzoxazole complexes of zirconium and hafnium: synthesis, structure and photo-physical behaviour.
Kuhlmann, Lisa; Methling, Rafael; Simon, Jasmin; Neumann, Beate; Stammler, Hans-Georg; Strassert, Cristian A.; Mitzel, Norbert W.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11245–11252; doi:10.1039/c8dt01757c

data_7047154
_publ_section_title
;
 Fluorescent phenoxy benzoxazole complexes of zirconium and hafnium:
 synthesis, structure and photo-physical behaviour.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11245
_journal_page_last               11252
_journal_paper_doi               10.1039/c8dt01757c
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C52 H32 N4 O8 Zr'
_chemical_formula_sum            'C52 H32 N4 O8 Zr'
_chemical_formula_weight         932.03
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-02-23
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2018-01-11 deposited with the CCDC.
2018-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.3990(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7490(2)
_cell_length_b                   14.56752(12)
_cell_length_c                   16.85932(16)
_cell_measurement_reflns_used    23857
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.2110
_cell_measurement_theta_min      4.0250
_cell_volume                     4032.39(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.0000
_diffrn_measured_fraction_theta_max 0.9993
_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      6.00  31.00   1.00   20.00    --   38.00  82.00 -41.63   25
  2  \w    -53.00 -13.00   1.00   20.00    --  -38.50 -57.00-180.00   40
  3  \w    -37.00 -12.00   1.00   20.00    --  -38.50 -77.00-180.00   25
  4  \w   -109.00 -20.00   1.00   20.00    --  -38.50 -38.00  60.00   89
  5  \w   -106.00 -13.00   1.00   20.00    --  -38.50 -57.00 -30.00   93
  6  \w    -75.00 -43.00   1.00   20.00    --  -38.50 -77.00-180.00   32
  7  \w   -109.00 -78.00   1.00   20.00    --  -38.50 -77.00-180.00   31
  8  \w     32.00  97.00   1.00   20.00    --   43.45-137.00  12.00   65
  9  \w     23.00  84.00   1.00   20.00    --   43.45-125.00-120.00   61
 10  \w    -25.00  72.00   1.00   20.00    --   43.45 -77.00  30.00   97
 11  \w     14.00  39.00   1.00   20.00    --   46.00  83.00-113.75   25
 12  \w     19.00  46.00   1.00   20.00    --   50.00  80.00  82.99   27
 13  \w     18.00  43.00   1.00   20.00    --   50.00  82.00 146.08   25
 14  \w     19.00  44.00   1.00   20.00    --   50.00  81.00-166.78   25
 15  \w     18.00  44.00   1.00   20.00    --   50.00  82.00 -11.59   26
 16  \w     32.00  59.00   1.00   20.00    --   62.00  76.00 120.42   27
 17  \w     94.00 125.00   1.00   20.00    --   62.00  76.00 120.42   31
 18  \w     36.00  67.00   1.00   20.00    --   66.00  75.00  19.17   31
 19  \w     36.00  63.00   1.00   20.00    --   66.00  75.00 -94.50   27
 20  \w    111.00 137.00   1.00   20.00    --   66.00  77.00  68.44   26
 21  \w    107.00 137.00   1.00   20.00    --   66.00  75.00  19.17   30
 22  \w     36.00 115.00   1.00   20.00    --   66.00  76.00 -63.16   79
 23  \w     36.00  64.00   1.00   20.00    --   66.00  77.00  68.44   28
 24  \w     39.00  65.00   1.00   20.00    --   66.00  66.00  -8.30   26
 25  \w     37.00  65.00   1.00   20.00    --   66.00  75.00-135.37   28
 26  \w     37.00  68.00   1.00   20.00    --   66.00  75.00-170.64   31
 27  \w     38.00  65.00   1.00   20.00    --   66.00  75.00 152.94   27
 28  \w     97.00 135.00   1.00   20.00    --   66.00  66.00  -8.30   38
 29  \w     49.00  79.00   1.00   63.00    --   78.00  75.00 113.99   30
 30  \w     49.00  75.00   1.00   63.00    --   78.00  72.00  -6.99   26
 31  \w     61.00  88.00   1.00   63.00    --   86.00  60.00 176.76   27
 32  \w     57.00  85.00   1.00   63.00    --   86.00  74.00   4.26   28
 33  \w     65.00 158.00   1.00   63.00    --   90.00  56.00 -95.18   93
 34  \w     64.00  90.00   1.00   63.00    --   90.00  60.00  79.58   26
 35  \w     66.00 120.00   1.00   63.00    --   94.00  68.00 140.50   54
 36  \w     67.00  94.00   1.00   63.00    --   94.00  70.00 178.21   27
 37  \w     67.00  95.00   1.00   63.00    --   94.00  63.00  90.00   28
 38  \w     72.00  97.00   1.00   63.00    --   98.00  65.00 155.48   25
 39  \w     50.00 132.00   1.00   63.00    --  111.00 -45.00 150.00   82
 40  \w     87.00 114.00   1.00   63.00    --  111.00  61.00-150.00   27
 41  \w     31.00  77.00   1.00   63.00    --  111.00 -94.00 -30.00   46
 42  \w     65.00 106.00   1.00   63.00    --  111.00 -94.00-150.00   41
 43  \w     31.00  89.00   1.00   63.00    --  111.00 -94.00-180.00   58
 44  \w     85.00 120.00   1.00   63.00    --  111.00  61.00 -60.00   35
 45  \w     85.00 119.00   1.00   63.00    --  111.00  61.00 -90.00   34
 46  \w    116.00 168.00   1.00   63.00    --  111.00  77.00   0.00   52
 47  \w     81.00 107.00   1.00   63.00    --  111.00  77.00   0.00   26
 48  \w    116.00 150.00   1.00   63.00    --  111.00  77.00  90.00   34
 49  \w     81.00 107.00   1.00   63.00    --  111.00  77.00  90.00   26
 50  \w     81.00 164.00   1.00   63.00    --  111.00  77.00 -30.00   83
 51  \w     81.00 150.00   1.00   63.00    --  111.00  77.00 -60.00   69
 52  \w     86.00 113.00   1.00   63.00    --  111.00  61.00  30.00   27
 53  \w    129.00 178.00   1.00   63.00    --  111.00  74.00-154.63   49
 54  \w     82.00 159.00   1.00   63.00    --  111.00  77.00  30.00   77
 55  \w     81.00 178.00   1.00   63.00    --  111.00  77.00 150.00   97
 56  \w     83.00 108.00   1.00   63.00    --  111.00  74.00-154.63   25
 57  \w     85.00 164.00   1.00   63.00    --  111.00  61.00-120.00   79
 58  \w     83.00 173.00   1.00   63.00    --  111.00  77.00  60.00   90
 59  \w    112.00 152.00   1.00   63.00    --  111.00  77.00-180.00   40
 60  \w     81.00 107.00   1.00   63.00    --  111.00  77.00-180.00   26
 61  \w     64.00 122.00   1.00   63.00    --  111.00-125.00 -30.00   58
 62  \w     81.00 176.00   1.00   63.00    --  111.00  77.00 -90.00   95
 63  \w     88.00 171.00   1.00   63.00    --  111.00  61.00 120.00   83
 64  \w     32.00  86.00   1.00   63.00    --  111.00 -94.00 120.00   54
 65  \w     40.00 104.00   1.00   63.00    --  111.00 -94.00   0.00   64
 66  \w     83.00 110.00   1.00   63.00    --  111.00  77.00-120.00   27
 67  \w     72.00 120.00   1.00   63.00    --  111.00-125.00-180.00   48
 68  \w     33.00 103.00   1.00   63.00    --  111.00 -94.00  60.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0091478000
_diffrn_orient_matrix_UB_12      0.0688806000
_diffrn_orient_matrix_UB_13      0.0669601000
_diffrn_orient_matrix_UB_21      0.0338363000
_diffrn_orient_matrix_UB_22      -0.0720951000
_diffrn_orient_matrix_UB_23      0.0648178000
_diffrn_orient_matrix_UB_31      0.0870164000
_diffrn_orient_matrix_UB_32      0.0352585000
_diffrn_orient_matrix_UB_33      0.0016963000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            40278
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.348
_diffrn_reflns_theta_min         4.057
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.789
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.102
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         3988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_R_factor_all          0.0221
_refine_ls_R_factor_gt           0.0207
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0187P)^2^+3.7676P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0505
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3824
_reflns_number_total             3988
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01757c2.cif
_cod_data_source_block           compound7
_cod_depositor_comments
'Adding full bibliography for 7047149--7047158.cif.'
_cod_original_cell_volume        4032.40(7)
_cod_database_code               7047154
_chemical_oxdiff_formula         'C52 H32 N4 O8 Zr'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_date_sample_data_collection 2016-02-19
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.756
_shelx_res_checksum              16636
_shelxl_version_number           2014-3