PCCP ligands with a semi-rigid backbone for chromium-catalyzed selective ethylene tri-/tetramerization
Zhao, Xing; Xie, Haojie; Zuo, Jing; Wang, Jihe; Zhao, Mei-Xin; Zhang, Jun; Catalysis Science & Technology 15 (2025) 2713–2721; doi:10.1039/D5CY00152H

data_1574059
_publ_section_title
;
 PCCP ligands with a semi-rigid backbone for chromium-catalyzed selective
 ethylene tri-/tetramerization
;
_journal_issue                   9
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              2713
_journal_page_last               2721
_journal_paper_doi               10.1039/D5CY00152H
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C33 H28 Cr O4 P2'
_chemical_formula_sum            'C33 H28 Cr O4 P2'
_chemical_formula_weight         602.49
_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
_audit_creation_date             2025-02-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2025-02-27 deposited with the CCDC.	2025-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.8800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6589(3)
_cell_length_b                   9.9032(2)
_cell_length_c                   14.3096(3)
_cell_measurement_reflns_used    7081
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.98
_cell_measurement_theta_min      3.35
_cell_volume                     1522.20(6)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0609
_diffrn_reflns_av_unetI/netI     0.0770
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15680
_diffrn_reflns_point_group_measured_fraction_full 0.856
_diffrn_reflns_point_group_measured_fraction_max 0.852
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.297
_diffrn_reflns_theta_min         3.352
_diffrn_source_current           1.1
_diffrn_source_power             0.055
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.370
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.570
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1481 before and 0.0982 after correction.
The Ratio of minimum to maximum transmission is 0.4261.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             624
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.294
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.050
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.058(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         4945
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0560
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0437P)^2^+0.5172P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1293
_reflns_Friedel_coverage         0.620
_reflns_Friedel_fraction_full    0.699
_reflns_Friedel_fraction_max     0.695
_reflns_number_gt                4399
_reflns_number_total             4945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cy00152h2.cif
_cod_data_source_block           cu_d8v23434_0m
_cod_depositor_comments
'Adding full bibliography for 1574058--1574059.cif.'
_cod_database_code               1574059
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.721
_shelx_estimated_absorpt_t_min   0.524
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.942(11)
 0.058(11)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uanis(C26) = Uanis(C25) = Uanis(C24)
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
4.b Aromatic/amide H refined with riding coordinates:
 C15(H15), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18),
 C19(H19), C20(H20), C21(H21), C27(H27), C23(H23), C24(H24), C26(H26), C29(H29),
  C30(H30), C31(H31), C32(H32), C33(H33)
4.c Fitted hexagon refined as free rotating group:
 C15(C10,C11,C12,C13,C14), C27(C22,C23,C24,C25,C26)
4.d Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              12478
_shelx_hkl_checksum              42699
_olex2_submission_special_instructions 'No special instructions were received'