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_2021845
_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 (C19 H32 O4 P)4 (C19 H33 O4 P)2 (O H)2], 2C7 H16'
_chemical_formula_moiety         'C114 H196 Cr2 O26 P6, 2(C7 H16)'
_chemical_formula_sum            'C128 H228 Cr2 O26 P6'
_chemical_formula_weight         2472.91
_chemical_name_systematic
;Bis(\m-butyl 2,6-di-<i>tert</i>-butyl-4-methylphenyl hydrogen phosphato-\k<i>O</i>:\k<i>O</i>')di-\m-hydroxido-bis[(butyl
2,6-di-<i>tert</i>-butyl-4-methylphenyl hydrogen phosphato-\k<i>O</i>)(butyl 2,6-di-<i>tert</i>-butyl-4-methylphenyl phosphato-\k<i>O</i>)chromium](<i>Cr</i>---<i>Cr</i>) heptane disolvate
;
_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   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 105.4430(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.0576(12)
_cell_length_b                   24.7423(19)
_cell_length_c                   18.2142(14)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.262
_cell_measurement_theta_min      2.138
_cell_volume                     6975.3(9)
_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      110(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_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  0.0295
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            59295
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.316
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.9445
_exptl_absorpt_correction_T_min  0.8932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.177
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2684
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.284
_refine_ls_abs_structure_details
;
Refined as an inversion twin
;
_refine_ls_abs_structure_Flack   0.330(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1541
_refine_ls_number_reflns         29623
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0541
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0634P)^2^+1.4487P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1118
_reflns_number_gt                25525
_reflns_number_total             29623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fp3081sup1.cif
_cod_data_source_block           mol1
_cod_depositor_comments
'Adding full bibliography for 2021845--2021847.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2021845
_cod_database_fobs_code          2021845
_shelx_estimated_absorpt_t_min   0.893
_shelx_estimated_absorpt_t_max   0.944
_shelx_hkl_checksum              62281
_shelx_res_checksum              60391