A tridentate phenoxy-phosphine (POP) divalent chromium complex and its reactivities in olefin polymerization
Ji, Li; Song, Ping; Zhou, Youyun; Sun, Xiu-Li; Gao, Yanshan; Tang, Yong; Polymer Chemistry 14 (2023) 763–772; doi:10.1039/D2PY01509A

data_1568328
_publ_section_title
;
 A tridentate phenoxy-phosphine (POP) divalent chromium complex and its
 reactivities in olefin polymerization
;
_journal_issue                   6
_journal_name_full               'Polymer Chemistry'
_journal_page_first              763
_journal_page_last               772
_journal_paper_doi               10.1039/D2PY01509A
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C42 H47 Cl3 Cr2 O3 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C50 H63 Cl3 Cr2 O5 P2'
_chemical_formula_weight         1016.29
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Light-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-09-04 deposited with the CCDC.	2023-01-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.481(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5840(9)
_cell_length_b                   13.1523(5)
_cell_length_c                   17.7764(7)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      68.33
_cell_measurement_theta_min      3.94
_cell_volume                     5044.7(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker PHOTON 100 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1106
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            53396
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.548
_diffrn_reflns_theta_min         3.936
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.11
_diffrn_source_power             0.0555
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.958
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.4039
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1259 before and 0.0712 after correction.
The Ratio of minimum to maximum transmission is 0.5363.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_F_000             2128
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.593
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         4633
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0564P)^2^+3.5872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4390
_reflns_number_total             4633
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2py01509a2.cif
_cod_data_source_block           cxy3236_0m
_cod_depositor_comments          'Adding full bibliography for 1568328.cif.'
_cod_database_code               1568328
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C24-C23 \\sim C24-C23A \\sim C23A-C22A \\sim C23-C22 \\sim C22-C21 \\sim
C22A-C21
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C22) = Uanis(C22A)
Uanis(C23) = Uanis(C23A)
4. Others
 Sof(H21C)=Sof(H21D)=Sof(H24C)=Sof(H24D)=Sof(C23A)=Sof(H23C)=Sof(H23D)=
 Sof(C22A)=Sof(H22C)=Sof(H22D)=1-FVAR(1)
 Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=
 Sof(H24A)=Sof(H24B)=FVAR(1)
 Fixed Sof: C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C12(0.5) H12A(0.5)
 H12B(0.5) H12C(0.5) C13(0.5) H13A(0.5) H13B(0.5) H13C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C21(H21C,H21D), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C24(H24C,H24D), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B),
 C28(H28A,H28B), C23A(H23C,H23D), C22A(H22C,H22D)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19)
5.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              45921
_olex2_submission_special_instructions 'No special instructions were received'