Synthesis, dynamics and redox properties of eight-coordinate zirconium catecholate complexes.
Do, Thomas H.; Brown, Seth N.; Dalton transactions (Cambridge, England : 2003) 49 (2020) 11648–11656; doi:10.1039/d0dt02487b

data_7705037
_publ_section_title
;
 Synthesis, dynamics and redox properties of eight-coordinate zirconium
 catecholate complexes.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11648
_journal_page_last               11656
_journal_paper_doi               10.1039/d0dt02487b
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C89 H82 N6 O5 Zr, 7(C4 H8 O)'
_chemical_formula_sum            'C117 H138 N6 O12 Zr'
_chemical_formula_weight         1911.55
_chemical_name_common            (TPP)Zr(XbicH2).7(THF)
_chemical_name_systematic
'Tetraphenylporphyrin-(9,9-dimethylxanthene-4,5-bis(iminium)bis(4,6-ditertbutylcatecholato))zirconium(IV) hepta-tetrahydrofuran solvate'
_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/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-07-12 deposited with the CCDC.	2020-08-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.6014(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.745(3)
_cell_length_b                   17.732(2)
_cell_length_c                   28.218(4)
_cell_measurement_reflns_used    9307
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.353
_cell_measurement_theta_min      2.277
_cell_volume                     9838(2)
_computing_cell_refinement       'Bruker SAINT (Bruker, 2015)'
_computing_data_collection       'Bruker APEX-3 (Bruker, 2015)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2015)'
_computing_molecular_graphics    'Bruker XP (Bruker, 2015)'
_computing_publication_material  'CIFTAB (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2014/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II'
_diffrn_measurement_method       'combination of \w and \f-scans '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            326985
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.453
_diffrn_reflns_theta_min         1.378
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.179
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
L. Krause, R. Herbst-Irmer, G. M. Sheldrick & D. Stalke. J. Appl.
Cryst., 2015, 48, 3.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4072
_exptl_crystal_recrystallization_method
;
Crystals deposited from THF at room temperature after 5 days. 
;
_exptl_crystal_size_max          0.409
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.192
_exptl_transmission_factor_max   0.745700
_exptl_transmission_factor_min   0.674300
_refine_diff_density_max         0.894
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1563
_refine_ls_number_reflns         24610
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0415P)^2^+11.7298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1024
_refine_ls_wR_factor_ref         0.1093
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19848
_reflns_number_total             24610
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02487b2.cif
_cod_data_source_block           TPPZrX
_cod_depositor_comments
'Adding full bibliography for 7705037--7705038.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7705037
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.930
_shelx_estimated_absorpt_t_max   0.966
_diffrn_source_monochromator     'Bruker TRIUMPH curved-graphite'
_shelx_res_checksum              67600