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_7047149
_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         'C32 H30 N2 O6 Zr'
_chemical_formula_sum            'C32 H30 N2 O6 Zr'
_chemical_formula_weight         629.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2015-11-11
_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                95.728(3)
_cell_angle_beta                 101.347(3)
_cell_angle_gamma                90.395(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7739(3)
_cell_length_b                   11.5955(4)
_cell_length_c                   12.7567(4)
_cell_measurement_reflns_used    45964
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      30.0710
_cell_measurement_theta_min      2.9020
_cell_volume                     1409.90(8)
_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
;
SHELXD, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9978
_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    -85.00   8.00   1.00    2.30    --  -17.00 -57.00 -60.00   93
  2  \w    -42.00  51.00   1.00    2.30    --  -17.00  57.00  60.00   93
  3  \w    -91.00 -39.00   1.00    2.30    --  -17.00 154.00 -30.47   52
  4  \w    -88.00   4.00   1.00    2.30    --  -17.00 -38.00  30.00   92
  5  \w    -13.00  89.00   1.00    2.30    --   17.39  77.00-180.00  102
  6  \w    -20.00  56.00   1.00    2.30    --   17.39 -99.00 -30.00   76
  7  \w    -13.00  89.00   1.00    2.30    --   17.39  77.00 -60.00  102
  8  \w    -20.00  56.00   1.00    2.30    --   17.39 -99.00 150.00   76
  9  \w    -54.00  48.00   1.00    2.30    --   17.39 -77.00-150.00  102
 10  \w    -91.00 -39.00   1.00    2.30    --  -17.00 154.00-116.26   52
 11  \w    -89.00 -37.00   1.00    2.30    --  -17.00 152.00 164.37   52
 12  \w    -76.00 -29.00   1.00    2.30    --  -17.00 133.00 121.11   47
 13  \w    -83.00 -34.00   1.00    2.30    --  -17.00 144.00  45.34   49
 14  \w    -88.00   4.00   1.00    2.30    --  -17.00 -38.00-180.00   92
 15  \w    -86.00 -35.00   1.00    2.30    --  -17.00 148.00-128.47   51
 16  \w    -54.00  38.00   1.00    2.30    --   17.39 -38.00 -60.00   92
 17  \w    -88.00 -37.00   1.00    2.30    --  -17.00 151.00 -67.51   51
 18  \w    -47.00  54.00   1.00    2.30    --  -17.00  77.00  90.00  101
 19  \w    -20.00  56.00   1.00    2.30    --   17.39 -99.00-150.00   76
 20  \w    -68.00 103.00   1.00    2.30    --   17.39   0.00-180.00  171
 21  \w    -68.00 103.00   1.00    2.30    --   17.39   0.00-150.00  171
 22  \w    -68.00   5.00   1.00    2.30    --   17.39   0.00-120.00   73
 23  \w     -3.00  68.00   1.00    2.30    --   17.39-119.00 167.38   71
;
_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      -0.0494595000
_diffrn_orient_matrix_UB_12      0.0011878000
_diffrn_orient_matrix_UB_13      -0.0486692000
_diffrn_orient_matrix_UB_21      -0.0261430000
_diffrn_orient_matrix_UB_22      0.0524258000
_diffrn_orient_matrix_UB_23      0.0209228000
_diffrn_orient_matrix_UB_31      0.0485054000
_diffrn_orient_matrix_UB_32      0.0320861000
_diffrn_orient_matrix_UB_33      -0.0210483000
_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  0.0421
_diffrn_reflns_av_unetI/netI     0.0200
_diffrn_reflns_Laue_measured_fraction_full 0.998
_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       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            83215
_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         29.997
_diffrn_reflns_theta_min         2.727
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.438
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.887
_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    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.225
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     374
_refine_ls_number_reflns         8218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0269P)^2^+0.7734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0605
_refine_ls_wR_factor_ref         0.0623
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7654
_reflns_number_total             8218
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01757c2.cif
_cod_data_source_block           compound1
_cod_depositor_comments
'Adding full bibliography for 7047149--7047158.cif.'
_cod_original_cell_volume        1409.90(9)
_cod_database_code               7047149
_chemical_oxdiff_formula         'C44 H62 N2 O10 Zr2'
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_date_sample_data_collection 2015-11-10
_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 1.336
_oxdiff_exptl_absorpt_empirical_full_min 0.725
_shelx_res_checksum              69023
_shelxl_version_number           2014-3