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_7047155
_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         'C40 H34 N2 O6 Zr'
_chemical_formula_sum            'C40 H34 N2 O6 Zr'
_chemical_formula_weight         729.91
_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             2016-02-05
_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                 94.3075(13)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   21.4580(3)
_cell_length_b                   18.0852(2)
_cell_length_c                   25.5064(4)
_cell_measurement_reflns_used    108020
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      30.0570
_cell_measurement_theta_min      1.6390
_cell_volume                     9870.4(2)
_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      air
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.9991
_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     -4.00  92.90   0.30    5.00    --   25.03  77.00 -30.00  323
  2  \w    -44.00  52.90   0.30    5.00    --   25.03 -77.00 -90.00  323
  3  \w    -43.00  44.00   0.30    5.00    --   25.03 -57.00  60.00  290
  4  \w     -4.00  92.90   0.30    5.00    --   25.03  77.00-150.00  323
  5  \w      7.00  91.90   0.30    5.00    --   25.03  57.00  90.00  283
  6  \w    -20.00  64.90   0.30    5.00    --   25.03 -99.00-180.00  283
  7  \w    -20.00  64.90   0.30    5.00    --   25.03 -99.00  30.00  283
  8  \w      7.00  91.90   0.30    5.00    --   25.03  57.00 120.00  283
  9  \w      3.00  96.00   0.30    5.00    --   25.03  38.00 -30.00  310
 10  \w    -46.00  47.00   0.30    5.00    --   25.03 -38.00-180.00  310
 11  \w    -47.00  61.90   0.30    5.00    --   25.03 -19.00 -60.00  363
 12  \w    -95.00  46.90   0.30    5.00    --  -23.50   0.00-180.00  473
 13  \w    -45.00   6.00   0.30    5.00    --  -23.50 -80.00 -21.00  170
 14  \w    -95.00  46.90   0.30    5.00    --  -23.50   0.00-120.00  473
 15  \w    -95.00  46.90   0.30    5.00    --  -23.50   0.00-150.00  473
 16  \w      7.00  91.90   0.30    5.00    --   25.03  57.00 -90.00  283
 17  \w      7.00  91.90   0.30    5.00    --   25.03  57.00-180.00  283
 18  \w    -20.00  64.90   0.30    5.00    --   25.03 -99.00  90.00  283
 19  \w    -20.00  64.90   0.30    5.00    --   25.03 -99.00 -90.00  283
 20  \w     -4.00  44.00   0.30    5.00    --   25.03  80.00 102.00  160
 21  \w    -95.00 -86.30   0.30    5.00    --  -23.50   0.00 -60.00   29
;
_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      0.0066161000
_diffrn_orient_matrix_UB_12      -0.0282051000
_diffrn_orient_matrix_UB_13      -0.0180831000
_diffrn_orient_matrix_UB_21      0.0146255000
_diffrn_orient_matrix_UB_22      0.0263729000
_diffrn_orient_matrix_UB_23      -0.0155832000
_diffrn_orient_matrix_UB_31      0.0289840000
_diffrn_orient_matrix_UB_32      -0.0068539000
_diffrn_orient_matrix_UB_33      0.0143757000
_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  0.0383
_diffrn_reflns_av_unetI/netI     0.0156
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            225130
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.079
_diffrn_reflns_theta_min         1.474
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.936
_exptl_absorpt_correction_T_min  0.891
_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_density_diffrn    1.474
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4512
_exptl_crystal_size_max          0.407
_exptl_crystal_size_mid          0.358
_exptl_crystal_size_min          0.197
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.757
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         14476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+12.9089P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0840
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13758
_reflns_number_total             14476
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01757c2.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 7047149--7047158.cif.'
_cod_database_code               7047155
_chemical_oxdiff_formula         'C40 H34 N2 O6 Zr'
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_date_sample_data_collection 2016-02-04
_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 1.296
_oxdiff_exptl_absorpt_empirical_full_min 0.767
_shelx_res_checksum              78365
_shelxl_version_number           2013-2