Benzylene-linked [PNP] scaffolds and their cyclometalated zirconium and hafnium complexes
Sietzen, Malte; Batke, Sonja; Antoni, Patrick W.; Wadepohl, Hubert; Ballmann, Joachim; Dalton Trans.  (2017) –; doi:10.1039/C7DT00413C

data_7042701
_publ_section_title
;
 Benzylene-linked [PNP] scaffolds and their cyclometalated zirconium and
 hafnium complexes
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT00413C
_journal_year                    2017
_chemical_formula_sum            'C52 H45 N P2 Zr'
_chemical_formula_weight         837.05
_chemical_properties_physical    'air-sensitive, moisture-sensitive'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_code                ba_jb32
_audit_creation_date             2016-08-05
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-03-17 deposited with the CCDC.
2017-04-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.1365(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.04739(15)
_cell_length_b                   12.35375(14)
_cell_length_c                   28.0234(3)
_cell_measurement_reflns_used    43081
_cell_measurement_temperature    120(1)
_cell_measurement_theta_max      31.7350
_cell_measurement_theta_min      3.2640
_cell_volume                     4814.17(9)
_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    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material
'encif (Wadepohl, 2009-15); encifer 1.5 (CCDC, 2014)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SUPERFLIP (Palatinus, 2007-2009)'
_diffrn_ambient_environment      perfluoro
_diffrn_ambient_temperature      120(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9621
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.974
_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    -41.00  50.00   0.50   12.50    --   28.16 -57.00 -60.00  182
  2  \w      7.00  97.00   0.50   12.50    --   28.16  57.00 -90.00  180
  3  \w    -20.00  72.00   0.50   12.50    --   28.16 -99.00-120.00  184
  4  \w      7.00  97.00   0.50   12.50    --   28.16  57.00   0.00  180
  5  \w      7.00  97.00   0.50   12.50    --   28.16  57.00  90.00  180
  6  \w    -20.00  72.00   0.50   12.50    --   28.16 -99.00  60.00  184
  7  \w     -6.00  23.00   0.50   12.50    --   28.16  82.00 -51.01   58
  8  \w    -41.00  50.00   0.50   12.50    --   28.16 -57.00 120.00  182
  9  \w      1.00 101.00   0.50   12.50    --   28.16  38.00-150.00  200
 10  \w     -5.00  24.00   0.50   12.50    --   28.16  80.00 145.92   58
 11  \w    -58.00 -27.00   0.50   12.50    --    4.00 132.00  51.95   62
 12  \w     -3.00  99.00   0.50   12.50    --   28.16  77.00-150.00  204
 13  \w    -20.00  72.00   0.50   12.50    --   28.16 -99.00  90.00  184
 14  \w     -3.00  99.00   0.50   12.50    --   28.16  77.00  60.00  204
 15  \w     -6.00  24.00   0.50   12.50    --   28.16  81.00  -4.40   60
 16  \w    -20.00  72.00   0.50   12.50    --   28.16 -99.00   0.00  184
 17  \w    -41.00  50.00   0.50   12.50    --   28.16 -57.00 150.00  182
 18  \w    -41.00  50.00   0.50   12.50    --   28.16 -57.00-150.00  182
 19  \w      1.00  44.00   0.50   12.50    --   28.16  38.00-120.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'polyimid foil'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0242983000
_diffrn_orient_matrix_UB_12      0.0120622000
_diffrn_orient_matrix_UB_13      -0.0233419000
_diffrn_orient_matrix_UB_21      -0.0297312000
_diffrn_orient_matrix_UB_22      -0.0460661000
_diffrn_orient_matrix_UB_23      0.0011361000
_diffrn_orient_matrix_UB_31      -0.0335633000
_diffrn_orient_matrix_UB_32      0.0320794000
_diffrn_orient_matrix_UB_33      0.0103845000
_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  0.0651
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            169444
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.344
_diffrn_reflns_theta_min         2.937
_diffrn_source                   'microfocus X-Ray tube'
_diffrn_source_type              'Agilent SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.327
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.947
_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            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.155
_exptl_crystal_description       needle
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.991
_refine_diff_density_min         -1.260
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     526
_refine_ls_number_reflns         16744
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0553
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0353P)^2^+5.0742P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15033
_reflns_number_total             16744
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt00413c2.cif
_cod_data_source_block           ba_jb32_sq
_cod_original_cell_volume        4814.18(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7042701
_audit_block_refno               2750
_audit_block_usercomment         'jb300, needle, orange'
_chemical_oxdiff_formula         'C63 H45 N P2 Zr'
_chemical_oxdiff_usercomment     'jb300, needle, orange'
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.968
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_shelxl_version_number           2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C23(H23), C24(H24),
  C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
 C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C48(H48), C49(H49), C50(H50), C51(H51), C52(H52)
;
_shelx_res_checksum              50212
_shelx_fab_checksum              28803
_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 1.184
_oxdiff_exptl_absorpt_empirical_full_min 0.788
_cell_oxdiff_length_a            14.05010(18)
_cell_oxdiff_length_b            12.35356(14)
_cell_oxdiff_length_c            28.0193(4)
_cell_oxdiff_angle_alpha         89.9704(10)
_cell_oxdiff_angle_beta          98.1485(11)
_cell_oxdiff_angle_gamma         90.0007(10)
_cell_oxdiff_volume              4814.18(11)
_cell_oxdiff_measurement_reflns_used 43081
_platon_squeeze_void_probe_radius 1.20