Chromium complexes bearing disubstituted organophosphate ligands and their use in ethylene polymerization
Tavtorkin, Alexander N.; Korchagina, Sof'ya A.; Komarov, Pavel D.; Vinogradov, Alexey A.; Churakov, Andrei V.; Nifant'ev, Ilya E.; Minyaev, Mikhail E.; Acta Crystallographica Section C 76 (2020) 93–103; doi:10.1107/S2053229619015699

data_2021846
_publ_section_title
;
 Chromium complexes bearing disubstituted organophosphate ligands and
 their use in ethylene polymerization
;
_journal_coeditor_code           FP3081
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              93
_journal_page_last               103
_journal_paper_doi               10.1107/S2053229619015699
_journal_volume                  76
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_iupac
'[Cr2 (C2 H5 O)2 (C24 H34 O4 P)3 Cl (C2 H6 O)3], C2 H6 O'
_chemical_formula_moiety         'C82 H130 Cl Cr2 O17 P3, C2 H6 O'
_chemical_formula_sum            'C84 H136 Cl Cr2 O18 P3'
_chemical_formula_weight         1666.28
_chemical_name_systematic
;[\m-Bis(2,6-diisopropylphenyl)
phosphato-1\k<i>O</i>:2\k<i>O</i>']bis[bis(2,6-diisopropylphenyl)
phosphato]-1\k<i>O</i>,2\k<i>O</i>-chlorido-2\k<i>Cl</i>-triethanol-1\k^2^<i>O</i>,2\k<i>O</i>-di-\m-ethanolato-1\k^2^<i>O</i>:2\k^2^<i>O</i>-dichromium(<i>Cr</i>---<i>Cr</i>) ethanol
monosolvate
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4994(10)
_cell_length_b                   23.1995(16)
_cell_length_c                   25.5787(17)
_cell_measurement_reflns_used    9369
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.588
_cell_measurement_theta_min      2.193
_cell_volume                     9197.5(11)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement
;
SHELXL2017 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0843
_diffrn_reflns_av_unetI/netI     0.0900
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            71757
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         2.193
_exptl_absorpt_coefficient_mu    0.379
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.9419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.499
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1037
_refine_ls_number_reflns         20083
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      0.960
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0496P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                13636
_reflns_number_total             20083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fp3081sup1.cif
_cod_data_source_block           mol2
_cod_depositor_comments
'Adding full bibliography for 2021845--2021847.cif.'
_cod_database_code               2021846
_cod_database_fobs_code          2021846
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.970
_shelx_hkl_checksum              56048
_shelx_res_checksum              73394