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_7047157
_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 Hf N4 O8'
_chemical_formula_sum            'C52 H32 Hf N4 O8'
_chemical_formula_weight         1019.30
_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             2016-12-15
_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                 101.3183(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.69585(13)
_cell_length_b                   14.60495(9)
_cell_length_c                   16.88832(11)
_cell_measurement_reflns_used    74717
_cell_measurement_temperature    99.8(4)
_cell_measurement_theta_max      30.0690
_cell_measurement_theta_min      1.8600
_cell_volume                     4037.99(5)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1901
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9997
_diffrn_measured_fraction_theta_max 0.9976
_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    -52.00  42.00   1.00    5.89    --  -28.55  57.00 -60.00   94
  2  \w    -52.00  42.00   1.00    5.89    --  -28.55  57.00-150.00   94
  3  \w   -111.00 -34.00   1.00    5.89    --  -28.55 178.00-180.00   77
  4  \w   -101.00   5.00   1.00    5.89    --  -28.55 -77.00  90.00  106
  5  \w    -99.00  -5.00   1.00    5.89    --  -28.55 -57.00 150.00   94
  6  \w    -99.00  -5.00   1.00    5.89    --  -28.55 -57.00 -30.00   94
  7  \w    -99.00  -5.00   1.00    5.89    --  -28.55 -57.00-120.00   94
  8  \w    -34.00  -5.00   1.00    5.89    --   28.62 129.00 -80.80   29
  9  \w    -20.00  73.00   1.00    5.89    --   28.62 -99.00  30.00   93
 10  \w     34.00 111.00   1.00    5.89    --   28.62-178.00-120.00   77
 11  \w    -47.00  95.00   1.00    5.89    --   28.62 -19.00   0.00  142
 12  \w   -101.00   5.00   1.00    5.89    --  -28.55 -77.00-180.00  106
 13  \w   -100.00 -53.00   1.00    5.89    --  -28.55-156.00 -79.00   47
 14  \w    -99.00  -5.00   1.00    5.89    --  -28.55 -57.00  30.00   94
 15  \w   -108.00 -35.00   1.00    5.89    --  -28.55-178.00-120.00   73
 16  \w     -3.00 102.00   1.00    5.89    --   28.62  38.00 -60.00  105
 17  \w    -20.00  73.00   1.00    5.89    --   28.62 -99.00-180.00   93
 18  \w     -4.00 101.00   1.00    5.89    --   28.62  77.00  30.00  105
 19  \w     -3.00 102.00   1.00    5.89    --   28.62  38.00  60.00  105
 20  \w    -34.00  -5.00   1.00    5.89    --   28.62 129.00-140.57   29
 21  \w    -46.00 104.00   1.00    5.89    --   28.62   0.00-150.00  150
 22  \w    -46.00 104.00   1.00    5.89    --   28.62   0.00-120.00  150
 23  \w    -46.00 104.00   1.00    5.89    --   28.62   0.00 -90.00  150
 24  \w    -46.00 104.00   1.00    5.89    --   28.62   0.00 -60.00  150
 25  \w    -46.00  92.00   1.00    5.89    --   28.62   0.00 -30.00  138
 26  \w    -46.00 104.00   1.00    5.89    --   28.62   0.00-180.00  150
;
_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      0.0060015000
_diffrn_orient_matrix_UB_12      0.0428305000
_diffrn_orient_matrix_UB_13      0.0200754000
_diffrn_orient_matrix_UB_21      -0.0123333000
_diffrn_orient_matrix_UB_22      0.0228902000
_diffrn_orient_matrix_UB_23      -0.0374493000
_diffrn_orient_matrix_UB_31      -0.0411076000
_diffrn_orient_matrix_UB_32      -0.0006293000
_diffrn_orient_matrix_UB_33      0.0053092000
_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  0.0396
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            117598
_diffrn_reflns_point_group_measured_fraction_full 0.999
_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         1.869
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.650
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.844
_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    1.677
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.314
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.138
_refine_diff_density_max         1.323
_refine_diff_density_min         -1.158
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         5945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0156
_refine_ls_R_factor_gt           0.0149
_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^)+(0.0148P)^2^+3.4952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0357
_refine_ls_wR_factor_ref         0.0361
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5781
_reflns_number_total             5945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01757c2.cif
_cod_data_source_block           compound9
_cod_depositor_comments
'Adding full bibliography for 7047149--7047158.cif.'
_cod_database_code               7047157
_chemical_oxdiff_formula         'C52 H32 O8 N4 Hf'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_date_sample_data_collection 2016-12-09
_olex2_date_sample_submission    1480978800
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7A) = Uanis(C46A) = Uanis(C20A) = Uanis(C33A)
3. Others
 Fixed Sof: O1A(0.5) C1A(0.5) C2A(0.5) H2A(0.5) C3A(0.5) H3A(0.5) C4A(0.5)
 H4A(0.5) C5A(0.5) H5A(0.5) C6A(0.5) C7A(0.5) O2A(0.5) C8A(0.5) C9A(0.5)
 H9A(0.5) C10A(0.5) H10A(0.5) C11A(0.5) H11A(0.5) C12A(0.5) H12A(0.5) C13A(0.5)
 N1A(0.5) O3A(0.5) C14A(0.5) C15A(0.5) H15A(0.5) C16A(0.5) H16A(0.5) C17A(0.5)
 H17A(0.5) C18A(0.5) H18A(0.5) C19A(0.5) C20A(0.5) O4A(0.5) C21A(0.5) C22A(0.5)
 H22A(0.5) C23A(0.5) H23A(0.5) C24A(0.5) H24A(0.5) C25A(0.5) H25A(0.5)
 C26A(0.5) N2A(0.5) O5A(0.5) C27A(0.5) C28A(0.5) H28A(0.5) C29A(0.5) H29A(0.5)
 C30A(0.5) H30A(0.5) C31A(0.5) H31A(0.5) C32A(0.5) C33A(0.5) O6A(0.5) C34A(0.5)
 C35A(0.5) H35A(0.5) C36A(0.5) H36A(0.5) C37A(0.5) H37A(0.5) C38A(0.5)
 H38A(0.5) C39A(0.5) N3A(0.5) O7A(0.5) C40A(0.5) C41A(0.5) H41A(0.5) C42A(0.5)
 H42A(0.5) C43A(0.5) H43A(0.5) C44A(0.5) H44A(0.5) C45A(0.5) C46A(0.5) O8A(0.5)
 C47A(0.5) C48A(0.5) H48A(0.5) C49A(0.5) H49A(0.5) C50A(0.5) H50A(0.5)
 C51A(0.5) H51A(0.5) C52A(0.5) N4A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C9A(H9A), C10A(H10A), C11A(H11A),
 C12A(H12A), C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A), C22A(H22A),
 C23A(H23A), C24A(H24A), C25A(H25A), C28A(H28A), C29A(H29A), C30A(H30A),
 C31A(H31A), C35A(H35A), C36A(H36A), C37A(H37A), C38A(H38A), C41A(H41A),
 C42A(H42A), C43A(H43A), C44A(H44A), C48A(H48A), C49A(H49A), C50A(H50A),
 C51A(H51A)
;
_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 1.328
_oxdiff_exptl_absorpt_empirical_full_min 0.681
_shelx_shelxl_version_number     2016/4