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_7047151
_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         'C48 H62 N2 O6 Zr'
_chemical_formula_sum            'C48 H62 N2 O6 Zr'
_chemical_formula_weight         854.21
_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             2017-09-27
_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                97.351(4)
_cell_angle_beta                 106.210(4)
_cell_angle_gamma                98.564(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5451(4)
_cell_length_b                   13.0261(6)
_cell_length_c                   17.4544(8)
_cell_measurement_reflns_used    9492
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      72.6710
_cell_measurement_theta_min      3.4550
_cell_volume                     2240.00(18)
_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 5.3114
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -78.00  17.00   1.00   20.00    --  -38.50 101.00 -38.00   95
  2  \w      4.00  66.00   1.00   20.00    --   42.95-101.00-142.00   62
  3  \w     76.00 112.00   1.00   49.00    --  111.00-101.00-142.00   36
  4  \w    139.00 178.00   1.00   49.00    --  111.00 101.00 -38.00   39
  5  \w   -109.00 -80.00   1.00   20.00    --  -38.50 -38.00  60.00   29
  6  \w    -51.00 -18.00   1.00   20.00    --  -38.50 -38.00  60.00   33
  7  \w    -57.00  32.00   1.00   20.00    --  -38.50  38.00 120.00   89
  8  \w     77.00 113.00   1.00   20.00    --   42.95  77.00   0.00   36
  9  \w     57.00 117.00   1.00   20.00    --   42.95 178.00-150.00   60
 10  \w     23.00  92.00   1.00   20.00    --   42.95  38.00-150.00   69
 11  \w      1.00  28.00   1.00   20.00    --   42.95 -99.00 -60.00   27
 12  \w     71.00  98.00   1.00   20.00    --   42.95  57.00-150.00   27
 13  \w     13.00 105.00   1.00   20.00    --   42.95  77.00  90.00   92
 14  \w     16.00 114.00   1.00   20.00    --   42.95  77.00 -60.00   98
 15  \w     19.00  52.00   1.00   20.00    --   42.95  57.00  60.00   33
 16  \w     19.00  47.00   1.00   20.00    --   42.95  57.00-150.00   28
 17  \w     17.00  55.00   1.00   20.00    --   42.95  77.00   0.00   38
 18  \w     76.00 110.00   1.00   20.00    --   42.95  57.00   0.00   34
 19  \w     13.00  50.00   1.00   20.00    --   42.95  77.00-180.00   37
 20  \w     59.00 109.00   1.00   20.00    --   42.95  57.00  60.00   50
 21  \w     18.00  46.00   1.00   20.00    --   42.95  57.00   0.00   28
 22  \w     15.00  92.00   1.00   20.00    --   42.95  77.00-120.00   77
 23  \w     45.00 135.00   1.00   49.00    --  111.00 -61.00-150.00   90
 24  \w     86.00 112.00   1.00   49.00    --  111.00  61.00 -30.00   26
 25  \w     85.00 111.00   1.00   49.00    --  111.00  61.00  90.00   26
 26  \w     87.00 127.00   1.00   49.00    --  111.00  61.00-150.00   40
 27  \w     82.00 108.00   1.00   49.00    --  111.00  77.00 120.00   26
 28  \w    116.00 171.00   1.00   49.00    --  111.00  77.00   0.00   55
 29  \w     82.00 109.00   1.00   49.00    --  111.00  72.00 -26.20   27
 30  \w     81.00 107.00   1.00   49.00    --  111.00  77.00  90.00   26
 31  \w    114.00 164.00   1.00   49.00    --  111.00  77.00  90.00   50
 32  \w     82.00 177.00   1.00   49.00    --  111.00  77.00-120.00   95
 33  \w     53.00 122.00   1.00   49.00    --  111.00-125.00  30.00   69
 34  \w     85.00 115.00   1.00   49.00    --  111.00  61.00  30.00   30
 35  \w     81.00 107.00   1.00   49.00    --  111.00  76.00-127.52   26
 36  \w     82.00 107.00   1.00   49.00    --  111.00  77.00   0.00   25
 37  \w     81.00 175.00   1.00   49.00    --  111.00  77.00 150.00   94
 38  \w     85.00 112.00   1.00   49.00    --  111.00  61.00 150.00   27
 39  \w    120.00 176.00   1.00   49.00    --  111.00  77.00-180.00   56
 40  \w    113.00 176.00   1.00   49.00    --  111.00  77.00  30.00   63
 41  \w     81.00 107.00   1.00   49.00    --  111.00  77.00-180.00   26
 42  \w     95.00 122.00   1.00   49.00    --  111.00-125.00-180.00   27
 43  \w     85.00 111.00   1.00   49.00    --  111.00  61.00-180.00   26
 44  \w     81.00 108.00   1.00   49.00    --  111.00  77.00  30.00   27
 45  \w     85.00 112.00   1.00   49.00    --  111.00  61.00-120.00   27
 46  \w     81.00 173.00   1.00   49.00    --  111.00  77.00-150.00   92
 47  \w     89.00 117.00   1.00   49.00    --  111.00  45.00  30.00   28
 48  \w     89.00 115.00   1.00   49.00    --  111.00  45.00 150.00   26
 49  \w     87.00 114.00   1.00   49.00    --  111.00  50.00-158.68   27
 50  \w     85.00 112.00   1.00   49.00    --  111.00  61.00 -90.00   27
 51  \w     81.00 107.00   1.00   49.00    --  111.00  77.00  60.00   26
 52  \w     43.00 141.00   1.00   49.00    --  111.00 -77.00  60.00   98
 53  \w     85.00 171.00   1.00   49.00    --  111.00  61.00 -60.00   86
 54  \w     82.00 178.00   1.00   49.00    --  111.00  72.00 -51.67   96
 55  \w     42.00  76.00   1.00   49.00    --  111.00-125.00-180.00   34
 56  \w     85.00 112.00   1.00   49.00    --  111.00  61.00  60.00   27
 57  \w    113.00 148.00   1.00   49.00    --  111.00  77.00 -90.00   35
 58  \w     81.00 107.00   1.00   49.00    --  111.00  77.00 -90.00   26
 59  \w     85.00 178.00   1.00   49.00    --  111.00  62.00  66.31   93
 60  \w     85.00 121.00   1.00   49.00    --  111.00  61.00   0.00   36
 61  \w     54.00 105.00   1.00   49.00    --  111.00 -94.00  30.00   51
 62  \w     85.00 174.00   1.00   49.00    --  111.00  61.00 120.00   89
;
_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      0.1473623000
_diffrn_orient_matrix_UB_12      0.0130472000
_diffrn_orient_matrix_UB_13      -0.0005195000
_diffrn_orient_matrix_UB_21      -0.0474024000
_diffrn_orient_matrix_UB_22      -0.0576071000
_diffrn_orient_matrix_UB_23      -0.0887988000
_diffrn_orient_matrix_UB_31      -0.0094008000
_diffrn_orient_matrix_UB_32      0.1062381000
_diffrn_orient_matrix_UB_33      -0.0290044000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0830
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35244
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.600
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_min         2.679
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.395
_exptl_absorpt_correction_T_max  0.995
_exptl_absorpt_correction_T_min  0.929
_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    1.266
_exptl_crystal_description       plate
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.163
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.937
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     530
_refine_ls_number_reflns         7924
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0578P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1155
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6451
_reflns_number_total             7924
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01757c2.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 7047149--7047158.cif.'
_cod_database_code               7047151
_chemical_oxdiff_formula         'C52 H59 N7'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.98
_olex2_date_sample_data_collection 2017-02-07
_olex2_date_sample_submission    1486335600
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C43(H43), C46(H46)
2.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)
2.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), C47(H47A,H47B,
 H47C), C48(H48A,H48B,H48C)
;
_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 1.512
_oxdiff_exptl_absorpt_empirical_full_min 0.684
_shelx_res_checksum              37823
_shelx_shelxl_version_number     2016/4