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_7716196
_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_absolute_configuration ad
_chemical_formula_moiety         'C36 H30 Br4 O2 P2 Zr'
_chemical_formula_sum            'C36 H30 Br4 O2 P2 Zr'
_chemical_formula_weight         967.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2dhp4r
_audit_creation_date             2022-09-13
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-11-14 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.875(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9980(3)
_cell_length_b                   15.5366(5)
_cell_length_c                   11.8659(3)
_cell_measurement_reflns_used    32941
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.62
_cell_measurement_theta_min      4.51
_cell_volume                     1810.09(9)
_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 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
 2620 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  0.0446
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23579
_diffrn_reflns_point_group_measured_fraction_full 0.936
_diffrn_reflns_point_group_measured_fraction_max 0.914
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         72.911
_diffrn_reflns_theta_min         3.793
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    8.743
_exptl_absorpt_correction_T_max  0.0270
_exptl_absorpt_correction_T_min  0.0084
_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    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_recrystallization_method
'The material was recrystallised from DCM by slow evaporation'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.08
_exptl_crystal_size_rad          0.090
_refine_diff_density_max         1.772
_refine_diff_density_min         -1.607
_refine_diff_density_rms         0.279
_refine_ls_abs_structure_details
;
 Flack x determined using 2197 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(4)
_refine_ls_extinction_coef       0.0083(7)
_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   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6613
_refine_ls_number_restraints     433
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0938
_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^)+(0.1000P)^2^+32.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2181
_refine_ls_wR_factor_ref         0.2455
_reflns_Friedel_coverage         0.777
_reflns_Friedel_fraction_full    0.868
_reflns_Friedel_fraction_max     0.832
_reflns_number_gt                5850
_reflns_number_total             6613
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01299b3.cif
_cod_data_source_block           cs153_150k
_cod_depositor_comments
'Adding full bibliography for 7716192--7716196.cif.'
_cod_database_code               7716196
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.541
_shelx_estimated_absorpt_t_min   0.054
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C8 \\sim C7 \\sim C12 \\sim C11 \\sim C10 \\sim C9: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C25 \\sim C30 \\sim C29 \\sim C28 \\sim C27 \\sim C26: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C14 \\sim C13 \\sim C18 \\sim C17 \\sim C16 \\sim C15: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6: within 2A with sigma of 0.04
and sigma for terminal atoms of 0.08 within 2A
C19 \\sim C24 \\sim C23 \\sim C22 \\sim C21 \\sim C20: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
C35 \\sim C36 \\sim C31 \\sim C32 \\sim C33 \\sim C34: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C13, C18, C17, C16, C15, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, C7, C12, C11, C10, C9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C24, C23, C22, C21, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C26, C27, C28, C29, C30, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C6, C1, C2, C3, C4, C5
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C31, C32, C33, C35, C34, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C32(H32), C36(H36), C6(H6), C26(H26), C35(H35), C30(H30), C20(H20),
 C3(H3), C29(H29), C9(H9), C34(H34), C33(H33), C14(H14), C24(H24), C8(H8),
 C12(H12), C10(H10), C23(H23), C22(H22), C11(H11), C5(H5), C16(H16), C4(H4),
 C18(H18), C21(H21), C28(H28), C17(H17), C27(H27), C15(H15)
;
_shelx_res_checksum              27184
_olex2_date_sample_data_collection 2022-09-10
_olex2_date_sample_submission    2022-09-05
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id CS153_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 0.017
_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 91.4
_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 145.9
_stoe_evaluation_lana_max_2theta_desired 145.9
_stoe_evaluation_lana_mean_redundancy 3.6
_stoe_evaluation_lana_number_refls_after_or 23593
_stoe_evaluation_lana_number_refls_outliers 8510
_stoe_evaluation_lana_number_refls_total 32103
_stoe_evaluation_lana_number_refls_unique 6621
_stoe_evaluation_lana_number_refls_written 23593
_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 2
_stoe_evaluation_lana_table
;
2Theta          14.3   29.9   45.5   61.1   76.7   92.3  107.9  123.5  139.1
<Resolution>    5.26   2.88   1.97   1.47   1.24   1.07   0.95   0.88   0.83
N(total)          70    452   1102   3740   6646   6903   4905   5414   2871
<Redundancy>     1.2    1.8    1.9    3.7    4.8    4.5    3.2    3.5    2.8
Complet. [%%]    91.2   96.8  100.0   98.3   98.6   95.2   89.8   88.6   75.0
<I/sigma>      136.8   84.9   55.1   28.4   23.4   17.9   12.5    9.4    5.5
R(int)         0.017  0.028  0.030  0.039  0.036  0.042  0.081  0.167  0.287
;
_stoe_measurement_identifier     CS153_150K
_stoe_measurement_max_exposure_per_frame '8.0 s'
_stoe_measurement_mean_exposure_per_frame '7.7 s'
_stoe_measurement_min_exposure_per_frame '2.0 s'
_stoe_measurement_total_exposure_time '5.6 h'
_stoe_measurement_total_frame_number 2620
_stoe_measurement_total_run_number 23
_stoe_measurement_tube_power     '50.0 W'