Complexation and disproportionation of group 4 metal (alkoxy) halides with phosphine oxides.
Seno, Carlotta; Pokratath, Rohan; Unniram Parambil, Ajmal Roshan; Van den Eynden, Dietger; Dhaene, Evert; Prescimone, Alessandro; De Roo, Jonathan; Dalton transactions (Cambridge, England : 2003) 53 (2024) 9862–9873; doi:10.1039/d4dt01299b

data_7716195
_publ_section_title
;
 Complexation and disproportionation of group 4 metal (alkoxy) halides
 with phosphine oxides.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9862
_journal_page_last               9873
_journal_paper_doi               10.1039/d4dt01299b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C36 H30 Cl4 Hf O2 P2'
_chemical_formula_sum            'C36 H30 Cl4 Hf O2 P2'
_chemical_formula_weight         876.83
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2dhp5s
_audit_creation_date             2023-11-14
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-23 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                101.253(2)
_cell_angle_beta                 108.000(2)
_cell_angle_gamma                92.173(3)
_cell_formula_units_Z            1
_cell_length_a                   9.4917(3)
_cell_length_b                   9.5535(3)
_cell_length_c                   10.5075(3)
_cell_measurement_reflns_used    30074
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.88
_cell_measurement_theta_min      4.54
_cell_volume                     883.81(5)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.186.0 (STOE, 2022)'
_computing_data_reduction
;
X-Area Integrate 2.5.3.0 (STOE, 2021)
X-Area LANA 2.7.5.0 (STOE, 2022)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'EIGER2 1M'
_diffrn_detector_area_resol_mean 13.33
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
 3641 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI Cu'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '1.2 0.6 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14940
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.121
_diffrn_reflns_theta_min         4.746
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    9.344
_exptl_absorpt_correction_T_max  0.0002
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.647
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.143
_exptl_crystal_size_min          0.11
_exptl_crystal_size_rad          0.140
_refine_diff_density_max         1.203
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.144
_refine_ls_extinction_coef       0.0032(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3442
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0600P)^2^+6.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3300
_reflns_number_total             3442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01299b3.cif
_cod_data_source_block           cs162_150k
_cod_depositor_comments
'Adding full bibliography for 7716192--7716196.cif.'
_cod_database_code               7716195
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.426
_shelx_estimated_absorpt_t_min   0.284
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C8(H8), C14(H14), C15(H15), C12(H12), C2(H2), C6(H6), C5(H5), C16(H16),
 C18(H18), C10(H10), C9(H9), C11(H11), C4(H4), C3(H3), C17(H17)
;
_shelx_res_checksum              77958
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_original_sample_id CS162_150K
_olex2_submission_special_instructions 'No special instructions were received'
_stoe_detector_distance          '40.0 mm'
_stoe_detector_pixelsize_x       '0.075 mm'
_stoe_detector_pixelsize_y       '0.075 mm'
_stoe_detector_size_x            '8.0 cm'
_stoe_detector_size_y            '7.7 cm'
_stoe_evaluation_integration_a   5.6
_stoe_evaluation_integration_b   -1.0
_stoe_evaluation_integration_ems 0.019
_stoe_evaluation_lana_bis_l_even_max -
_stoe_evaluation_lana_bis_l_odd_max -
_stoe_evaluation_lana_bos_l_even_max 6
_stoe_evaluation_lana_bos_l_odd_max 3
_stoe_evaluation_lana_completeness 97.4
_stoe_evaluation_lana_dxs_max_order 1
_stoe_evaluation_lana_dys_max_order 1
_stoe_evaluation_lana_fs_max_order 3
_stoe_evaluation_lana_max_2theta_available 146.3
_stoe_evaluation_lana_max_2theta_desired 146.3
_stoe_evaluation_lana_mean_redundancy 4.3
_stoe_evaluation_lana_number_refls_after_or 14943
_stoe_evaluation_lana_number_refls_outliers 6335
_stoe_evaluation_lana_number_refls_total 21278
_stoe_evaluation_lana_number_refls_unique 3445
_stoe_evaluation_lana_number_refls_written 14943
_stoe_evaluation_lana_or_c1      0.035
_stoe_evaluation_lana_or_c2      0
_stoe_evaluation_lana_or_c3      0
_stoe_evaluation_lana_or_c4      0.7
_stoe_evaluation_lana_point_group -1
_stoe_evaluation_lana_table
;
2Theta          16.1   31.5   46.9   62.3   77.7   93.1  108.5  123.9  139.3
<Resolution>    4.69   2.71   1.92   1.46   1.23   1.07   0.95   0.87   0.83
N(total)          64    348    920   2706   4693   4460   3280   3151   1656
<Redundancy>     1.5    2.4    2.8    5.1    6.5    5.3    3.8    3.7    2.8
Complet. [%%]    97.4  100.0  100.0   99.7  100.0  100.0   99.0   98.5   84.6
<I/sigma>      245.2  121.1   97.8   51.6   37.8   32.6   23.4   16.0    8.8
R(int)         0.016  0.019  0.017  0.023  0.025  0.028  0.055  0.125  0.216
;
_stoe_measurement_identifier     CS162_150K
_stoe_measurement_max_exposure_per_frame '6.0 s'
_stoe_measurement_mean_exposure_per_frame '5.8 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '5.9 h'
_stoe_measurement_total_frame_number 3641
_stoe_measurement_total_run_number 34
_stoe_measurement_tube_power     '50.0 W'