Arrested disproportionation in trivalent, mononuclear, and non-metallocene complexes of Zr(iii) and Hf(iii).
Grant, Lauren N.; Miehlich, Matthias E.; Meyer, Karsten; Mindiola, Daniel J.; Chemical communications (Cambridge, England) 54 (2018) 2052–2055; doi:10.1039/c7cc08815a

data_7121194
_publ_section_title
;
 Arrested disproportionation in trivalent, mononuclear, and
 non-metallocene complexes of Zr(iii) and Hf(iii).
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              2052
_journal_page_last               2055
_journal_paper_doi               10.1039/c7cc08815a
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C44 H62 Cl N2 P2 Zr'
_chemical_formula_sum            'C44 H62 Cl N2 P2 Zr'
_chemical_formula_weight         807.56
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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Olex2 1.2
(compiled Jan 19 2015 12:28:14 for OlexSys, GUI svn.r4998)
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_audit_update_record
;
2017-10-27 deposited with the CCDC.
2018-01-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.9610(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.7014(6)
_cell_length_b                   13.7831(5)
_cell_length_c                   17.8222(7)
_cell_measurement_reflns_used    9195
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.527
_cell_measurement_theta_min      2.995
_cell_volume                     4282.7(3)
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Bruker APEX3 v2016.1-0
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Bruker SAINT v8.37A
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'shelXT v2014/5'
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_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0180
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            94375
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.568
_diffrn_reflns_theta_min         2.956
_diffrn_source                   'sealed tube'
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_exptl_absorpt_coefficient_mu    0.425
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_exptl_absorpt_correction_type   multi-scan
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;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0530 before and 0.0492 after correction.
The Ratio of minimum to maximum transmission is 0.9405.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_description       plate
_exptl_crystal_F_000             1708
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.25
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_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+6.1753P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1068
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8768
_reflns_number_total             9863
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_depositor_comments
'Adding full bibliography for 7121193--7121196.cif.'
_cod_database_code               7121194
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'