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_7716193
_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         'C8 H16 Br4 O2 Zr'
_chemical_formula_sum            'C8 H16 Br4 O2 Zr'
_chemical_formula_weight         555.07
_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.cc2dhp6t
_audit_creation_date             2022-10-03
_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                87.085(8)
_cell_angle_beta                 68.311(8)
_cell_angle_gamma                71.788(8)
_cell_formula_units_Z            1
_cell_length_a                   7.1420(7)
_cell_length_b                   7.5304(8)
_cell_length_c                   8.0799(8)
_cell_measurement_reflns_used    7773
_cell_measurement_temperature    150
_cell_measurement_theta_max      71.50
_cell_measurement_theta_min      5.91
_cell_volume                     382.53(7)
_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 0.990
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_details
;
 3719 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           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6412
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         73.062
_diffrn_reflns_theta_min         7.312
_diffrn_source                   'Axo Cu'
_diffrn_source_current           1.00
_diffrn_source_power             0.050
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    17.995
_exptl_absorpt_correction_T_max  0.0000
_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    2.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             260
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.07
_exptl_crystal_size_rad          0.180
_refine_diff_density_max         1.089
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.204
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1496
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0846
_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^+4.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1752
_refine_ls_wR_factor_ref         0.1949
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1079
_reflns_number_total             1496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01299b3.cif
_cod_data_source_block           por195_150k
_cod_depositor_comments
'Adding full bibliography for 7716192--7716196.cif.'
_cod_database_code               7716193
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.366
_shelx_estimated_absorpt_t_min   0.089
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
O1 \\sim C4 \\sim C3 \\sim C2 \\sim C1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
3. Rigid body (RIGU) restrains
 C1, C2, C3, C4, O1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C2(H2A,H2B), C4(H4A,H4B), C1(H1A,H1B)
;
_shelx_res_checksum              93114
_olex2_date_sample_data_collection 2022-09-30
_olex2_date_sample_submission    2022-09-16
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in perfluoroether oil'
_olex2_submission_original_sample_id POR195_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 98.2
_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 146.2
_stoe_evaluation_lana_max_2theta_desired 146.2
_stoe_evaluation_lana_mean_redundancy 4.3
_stoe_evaluation_lana_number_refls_after_or 6422
_stoe_evaluation_lana_number_refls_outliers 2741
_stoe_evaluation_lana_number_refls_total 9163
_stoe_evaluation_lana_number_refls_unique 1501
_stoe_evaluation_lana_number_refls_written 6422
_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          19.3   34.3   49.3   64.3   79.3   94.3  109.3  124.3  139.3
<Resolution>    4.14   2.55   1.83   1.42   1.21   1.06   0.94   0.87   0.83
N(total)          59    231    412   1289   1814   1743   1426   1401    788
<Redundancy>     2.2    2.8    2.4    5.2    5.8    4.7    4.1    4.1    3.4
Complet. [%%]   100.0  100.0  100.0  100.0   99.5   99.6   99.2   98.4   90.4
<I/sigma>      197.8  125.4   86.0   31.5   25.9   15.7    7.7    2.6    0.8
R(int)         0.035  0.028  0.030  0.072  0.065  0.088  0.153  0.366  0.481
;
_stoe_measurement_identifier     POR195_150K
_stoe_measurement_max_exposure_per_frame '2.0 s'
_stoe_measurement_mean_exposure_per_frame '1.9 s'
_stoe_measurement_min_exposure_per_frame '1.0 s'
_stoe_measurement_total_exposure_time '2.0 h'
_stoe_measurement_total_frame_number 3719
_stoe_measurement_total_run_number 33
_stoe_measurement_tube_power     '50.0 W'