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_7716194
_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 O2 P2 Zr'
_chemical_formula_sum            'C36 H30 Cl4 O2 P2 Zr'
_chemical_formula_weight         789.56
_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.cc2dhp1n
_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                101.126(3)
_cell_angle_beta                 107.899(3)
_cell_angle_gamma                92.429(3)
_cell_formula_units_Z            1
_cell_length_a                   9.4661(4)
_cell_length_b                   9.5612(4)
_cell_length_c                   10.5356(4)
_cell_measurement_reflns_used    34110
_cell_measurement_temperature    150
_cell_measurement_theta_max      73.15
_cell_measurement_theta_min      4.52
_cell_volume                     885.05(7)
_computing_cell_refinement       'X-Area Recipe 1.37.0.0 (STOE, 2021)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.175.0 (STOE, 2021)'
_computing_data_reduction
;
X-Area Integrate 2.5.1.0 (STOE, 2021)
X-Area LANA 2.6.2.0 (STOE, 2021)
;
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_details
;
 4262 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_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           GaK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16749
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.804
_diffrn_reflns_theta_min         4.518
_diffrn_source                   'Axo Cu'
_diffrn_source_current           3.570
_diffrn_source_power             0.250
_diffrn_source_voltage           70
_exptl_absorpt_coefficient_mu    6.427
_exptl_absorpt_correction_T_max  0.0017
_exptl_absorpt_correction_T_min  0.0003
_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    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.157
_exptl_crystal_size_min          0.15
_exptl_crystal_size_rad          0.150
_refine_diff_density_max         1.145
_refine_diff_density_min         -1.273
_refine_diff_density_rms         0.148
_refine_ls_extinction_coef       0.0187(13)
_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   0.903
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3432
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0840
_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^)+(0.0400P)^2^+9.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1668
_refine_ls_wR_factor_ref         0.1820
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3120
_reflns_number_total             3432
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01299b3.cif
_cod_data_source_block           cs145_150k
_cod_depositor_comments
'Adding full bibliography for 7716192--7716196.cif.'
_cod_original_cell_volume        885.05(6)
_cod_database_code               7716194
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.446
_shelx_estimated_absorpt_t_min   0.408
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C14(H14), C2(H2), C6(H6), C5(H5), C16(H16), C8(H8), C17(H17), C3(H3),
 C11(H11), C12(H12), C9(H9), C15(H15), C18(H18), C10(H10)
;
_shelx_res_checksum              53278
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_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 0.017
_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 145.7
_stoe_evaluation_lana_max_2theta_desired 145.7
_stoe_evaluation_lana_mean_redundancy 4.9
_stoe_evaluation_lana_number_refls_after_or 16758
_stoe_evaluation_lana_number_refls_outliers 7115
_stoe_evaluation_lana_number_refls_total 23873
_stoe_evaluation_lana_number_refls_unique 3437
_stoe_evaluation_lana_number_refls_written 16758
_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          15.8   31.2   46.6   62.0   77.4   92.8  108.2  123.6  139.0
<Resolution>    4.53   2.72   1.94   1.47   1.23   1.07   0.95   0.87   0.83
N(total)          98    611   1229   2855   5381   5010   3521   3303   1865
<Redundancy>     2.1    3.7    3.5    5.5    7.4    6.0    4.1    4.0    3.4
Complet. [%%]    97.4  100.0  100.0  100.0  100.0   99.7   99.5   97.3   85.5
<I/sigma>      247.0  120.3   89.2   47.8   34.2   29.9   21.2   12.3    6.0
R(int)         0.021  0.026  0.027  0.033  0.035  0.037  0.057  0.151  0.283
;
_stoe_measurement_identifier     CS145_150K
_stoe_measurement_max_exposure_per_frame '8.0 s'
_stoe_measurement_mean_exposure_per_frame '6.3 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '7.5 h'
_stoe_measurement_total_frame_number 4262
_stoe_measurement_total_run_number 71
_stoe_measurement_tube_power     '50.0 W'