Inducing selectivity and chirality in group IV metal coordination with high-denticity hydroxypyridinones.
Deblonde, Gauthier J.-P.; Lohrey, Trevor D.; Abergel, Rebecca J.; Dalton transactions (Cambridge, England : 2003) 48 (2019) 8238–8247; doi:10.1039/c9dt01031a

data_7700007
_publ_section_title
;
 Inducing selectivity and chirality in group IV metal coordination with
 high-denticity hydroxypyridinones.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8238
_journal_page_last               8247
_journal_paper_doi               10.1039/c9dt01031a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C34 H34 Hf N8 O12, 3(H2 O)'
_chemical_formula_sum            'C34 H40 Hf N8 O15'
_chemical_formula_weight         979.23
_chemical_name_common            'Hf(3,4,3-HOPO) trihydrate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2019-04-06 deposited with the CCDC.    2019-05-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_a                   16.0989(7)
_cell_length_b                   16.9738(7)
_cell_length_c                   13.3829(6)
_cell_measurement_reflns_used    23773
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.666
_cell_measurement_theta_min      2.523
_cell_volume                     3657.0(3)
_computing_cell_refinement       'SAINT V8.38A Bruker, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker, Madison WI'
_computing_molecular_graphics    ORTEP-32
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23773
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        27.710
_diffrn_reflns_theta_max         33.666
_diffrn_reflns_theta_min         2.523
_diffrn_source                   'Advanced Light Source, station 11.3.1'
_exptl_absorpt_coefficient_mu    3.646
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.6717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       shard
_exptl_crystal_F_000             1968
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.997
_refine_diff_density_min         -1.282
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details
;
 Flack x determined using 2381 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.026(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     296
_refine_ls_number_reflns         5551
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0176
_refine_ls_shift/su_max          0.068
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0075P)^2^+4.7122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0458
_refine_ls_wR_factor_ref         0.0461
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.968
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                5436
_reflns_number_total             5551
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01031a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7700007.cif.
;
_cod_database_code               7700007
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.712
_shelx_estimated_absorpt_t_max   0.811
_shelx_res_checksum              84483