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_7047150
_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         'C34 H34 Hf N2 O6'
_chemical_formula_sum            'C34 H34 Hf N2 O6'
_chemical_formula_weight         745.12
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-09-26
_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                 95.7585(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.70835(7)
_cell_length_b                   17.17797(14)
_cell_length_c                   18.59264(14)
_cell_measurement_reflns_used    83134
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      30.0810
_cell_measurement_theta_min      1.6160
_cell_volume                     3085.04(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9979
_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  83.00   1.00    2.00    --   24.87-131.00 -54.95   77
  2  \w    -46.00  96.00   1.00    2.00    --   24.87   0.00-120.00  142
  3  \w     -4.00  94.00   1.00    2.00    --   24.87  77.00 -30.00   98
  4  \w      6.00  93.00   1.00    2.00    --   24.87  57.00  90.00   87
  5  \w      3.00  95.00   1.00    2.00    --   24.87  38.00 -60.00   92
  6  \w     35.00  99.00   1.00    2.00    --   24.87 178.00 150.00   64
  7  \w     -4.00  94.00   1.00    2.00    --   24.87  77.00-180.00   98
  8  \w    -46.00  47.00   1.00    2.00    --   24.87 -38.00-180.00   93
  9  \w    -20.00  65.00   1.00    2.00    --   24.87 -99.00 150.00   85
 10  \w      7.00  85.00   1.00    2.00    --   24.87-133.00  40.38   78
 11  \w    -85.00  -8.00   1.00    2.00    --  -23.50 135.00  82.14   77
 12  \w    -97.00 -35.00   1.00    2.00    --  -23.50-178.00  90.00   62
 13  \w    -95.00  48.00   1.00    2.00    --  -23.50   0.00-180.00  143
 14  \w     -4.00  94.00   1.00    2.00    --   24.87  77.00-150.00   98
 15  \w      6.00  93.00   1.00    2.00    --   24.87  57.00  30.00   87
 16  \w    -46.00  47.00   1.00    2.00    --   24.87 -38.00 -90.00   93
 17  \w     -4.00  94.00   1.00    2.00    --   24.87  77.00  90.00   98
 18  \w      6.00  93.00   1.00    2.00    --   24.87  57.00 -60.00   87
 19  \w    -95.00  48.00   1.00    2.00    --  -23.50   0.00-120.00  143
 20  \w    -95.00  48.00   1.00    2.00    --  -23.50   0.00 -90.00  143
 21  \w    -95.00  48.00   1.00    2.00    --  -23.50   0.00 -60.00  143
 22  \w    -95.00  48.00   1.00    2.00    --  -23.50   0.00 -30.00  143
 23  \w    -95.00  48.00   1.00    2.00    --  -23.50   0.00-150.00  143
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0519449000
_diffrn_orient_matrix_UB_12      0.0209445000
_diffrn_orient_matrix_UB_13      0.0214913000
_diffrn_orient_matrix_UB_21      0.0507184000
_diffrn_orient_matrix_UB_22      -0.0144179000
_diffrn_orient_matrix_UB_23      -0.0215039000
_diffrn_orient_matrix_UB_31      -0.0109824000
_diffrn_orient_matrix_UB_32      0.0325270000
_diffrn_orient_matrix_UB_33      -0.0233771000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0166
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            177072
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.9674
_diffrn_reflns_theta_max         30.1135
_diffrn_reflns_theta_min         1.618
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.429
_exptl_absorpt_correction_T_max  0.922
_exptl_absorpt_correction_T_min  0.811
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.604
_exptl_crystal_description       column
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.336
_exptl_crystal_size_mid          0.231
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.913
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         9067
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0210
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0074P)^2^+4.3826P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0434
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8603
_reflns_number_total             9067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01757c2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
'Adding full bibliography for 7047149--7047158.cif.'
_cod_database_code               7047150
_chemical_oxdiff_formula         'C34 H34 Hf N2 O6'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.97
_olex2_date_sample_data_collection 2016-09-23
_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 1.285
_oxdiff_exptl_absorpt_empirical_full_min 0.841
_shelx_res_checksum              45484
_shelxl_version_number           2013-2