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_7047158
_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         'C50 H66 Hf N2 O6, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C50.5 H67 Cl Hf N2 O6'
_chemical_formula_weight         1012.00
_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     direct
_audit_creation_date             2016-10-06
_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                91.5475(6)
_cell_angle_beta                 91.2308(7)
_cell_angle_gamma                98.6382(7)
_cell_formula_units_Z            2
_cell_length_a                   10.62492(9)
_cell_length_b                   13.18535(10)
_cell_length_c                   17.81500(14)
_cell_measurement_reflns_used    93678
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      31.8970
_cell_measurement_theta_min      2.2290
_cell_volume                     2465.73(3)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0951
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9999
_diffrn_measured_fraction_theta_max 0.9424
_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  96.00   1.00   10.00    --   25.97  77.00  60.00  100
  2  \w    -44.00  56.00   1.00   10.00    --   25.97 -77.00-150.00  100
  3  \w     -4.00  96.00   1.00   10.00    --   25.97  77.00 -30.00  100
  4  \w    -44.00  56.00   1.00   10.00    --   25.97 -77.00 120.00  100
  5  \w     -4.00  96.00   1.00   10.00    --   25.97  77.00-180.00  100
  6  \w      0.00  98.00   1.00   10.00    --   25.97  38.00-180.00   98
  7  \w     -4.00  96.00   1.00   10.00    --   25.97  77.00-120.00  100
  8  \w    -20.00  68.00   1.00   10.00    --   25.97 -99.00 -30.00   88
  9  \w    -20.00  68.00   1.00   10.00    --   25.97 -99.00  60.00   88
 10  \w    -99.00 -35.00   1.00   10.00    --  -23.50-178.00 -30.00   64
 11  \w    -92.00  -2.00   1.00   10.00    --  -23.50 -57.00  30.00   90
 12  \w    -20.00  68.00   1.00   10.00    --   25.97 -99.00 150.00   88
 13  \w      0.00  98.00   1.00   10.00    --   25.97  38.00 -30.00   98
 14  \w    -43.00  47.00   1.00   10.00    --   25.97 -57.00 -60.00   90
 15  \w    -47.00  99.00   1.00   10.00    --   25.97   0.00-180.00  146
 16  \w    -46.00  51.00   1.00   10.00    --   25.97 -38.00   0.00   97
 17  \w    -46.00  51.00   1.00   10.00    --   25.97 -38.00-150.00   97
 18  \w    -47.00  99.00   1.00   10.00    --   25.97   0.00-120.00  146
 19  \w    -47.00  99.00   1.00   10.00    --   25.97   0.00 -90.00  146
 20  \w    -47.00  99.00   1.00   10.00    --   25.97   0.00 -60.00  146
 21  \w    -47.00  99.00   1.00   10.00    --   25.97   0.00 -30.00  146
 22  \w    -47.00  57.00   1.00   10.00    --   25.97   0.00   0.00  104
 23  \w    -47.00  99.00   1.00   10.00    --   25.97   0.00-150.00  146
;
_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      0.0502222000
_diffrn_orient_matrix_UB_12      0.0141440000
_diffrn_orient_matrix_UB_13      0.0268782000
_diffrn_orient_matrix_UB_21      -0.0133566000
_diffrn_orient_matrix_UB_22      0.0511276000
_diffrn_orient_matrix_UB_23      0.0008882000
_diffrn_orient_matrix_UB_31      -0.0431496000
_diffrn_orient_matrix_UB_32      -0.0122200000
_diffrn_orient_matrix_UB_33      0.0293973000
_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  0.0362
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            144424
_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         1.563
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.217
_exptl_absorpt_correction_T_max  0.932
_exptl_absorpt_correction_T_min  0.790
_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    1.363
_exptl_crystal_description       plate
_exptl_crystal_F_000             1042
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.552
_refine_diff_density_min         -0.907
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     607
_refine_ls_number_reflns         14456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.123
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0199
_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^)+(0.0222P)^2^+1.9476P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0501
_refine_ls_wR_factor_ref         0.0506
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13944
_reflns_number_total             14456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01757c2.cif
_cod_data_source_block           compound6
_cod_depositor_comments
'Adding full bibliography for 7047149--7047158.cif.'
_cod_original_formula_sum        'C50.50 H67 Cl Hf N2 O6'
_cod_database_code               7047158
_chemical_oxdiff_formula         'C50 H67 Cl N2 Hf O6'
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.01
_olex2_date_sample_data_collection 2016-09-30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: C48(0.5) H48A(0.5) H48B(0.5) H48C(0.5) C48B(0.5) H48D(0.5)
 H48E(0.5) H48F(0.5) C49(0.5) H49A(0.5) H49B(0.5) H49C(0.5) C49B(0.5) H49D(0.5)
 H49E(0.5) H49F(0.5) C50(0.5) H50A(0.5) H50B(0.5) H50C(0.5) C50B(0.5) H50D(0.5)
 H50E(0.5) H50F(0.5) Cl1(0.5) Cl2(0.5) C51(0.5) H51A(0.5) H51B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C10(H10), C11(H11), C12(H12), C24(H24), C26(H26),
 C30(H30), C31(H31), C32(H32), C33(H33)
3.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C36(H36A,H36B,H36C), C37(H37A,
 H37B,H37C), C38(H38A,H38B,H38C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C42(H42A,H42B,H42C), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C), C46(H46A,H46B,
 H46C), C48(H48A,H48B,H48C), C48B(H48D,H48E,H48F), C49(H49A,H49B,H49C),
 C49B(H49D,H49E,H49F), C50(H50A,H50B,H50C), C50B(H50D,H50E,H50F)
;
_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 1.298
_oxdiff_exptl_absorpt_empirical_full_min 0.792
_shelxl_version_number           2013-3