Highly active chromium-based selective ethylene tri-/tetramerization catalysts supported by alkenylphosphanyl PNP ligands.
Zhou, Tao; Zuo, Jing; Xie, Haojie; Zhao, Xing; Zhao, Mei-Xin; Zhang, Jun; Dalton transactions (Cambridge, England : 2003) 53 (2024) 14011–14017; doi:10.1039/d4dt01521e

data_7716799
_publ_section_title
;
 Highly active chromium-based selective ethylene tri-/tetramerization
 catalysts supported by alkenylphosphanyl PNP ligands.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14011
_journal_page_last               14017
_journal_paper_doi               10.1039/d4dt01521e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '2(C24 H29 Cr N O4 P2)'
_chemical_formula_sum            'C48 H58 Cr2 N2 O8 P4'
_chemical_formula_weight         1018.84
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-10 deposited with the CCDC.	2024-07-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.2300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4047(3)
_cell_length_b                   30.1693(10)
_cell_length_c                   18.1546(7)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      23.960
_cell_measurement_theta_min      2.261
_cell_volume                     5110.1(3)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      213.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0739
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43789
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.320
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.602
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6909
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1131 before and 0.0677 after correction.
The Ratio of minimum to maximum transmission is 0.9266.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             2128
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: 1-hexane/toluene'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.364
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     869
_refine_ls_number_reflns         8975
_refine_ls_number_restraints     1011
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^+10.0438P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1562
_refine_ls_wR_factor_ref         0.1846
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5680
_reflns_number_total             8975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt01521e2.cif
_cod_data_source_block           mo_d8v23674_0m
_cod_depositor_comments          'Adding full bibliography for 7716799.cif.'
_cod_database_code               7716799
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.910
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C48-C46 = C47-C46
 1.52 with sigma of 0.01
 C65-C63 = C64-C63
 1.52 with sigma of 0.01
 C24-C22 = C23-C22 = C21-C20
 1.52 with sigma of 0.01
 C47-C46 = C48-C46
 1.52 with sigma of 0.01
 C23-C22 = C24-C22
 1.52 with sigma of 0.01
 C17-N1 = C17-C18A = C17-C19A = C17-C18 = C17-C19
 1.52 with sigma of 0.01
 C62-C61
 1.52 with sigma of 0.01
 C45-C44
 1.52 with sigma of 0.01
 C21-C20
 1.52 with sigma of 0.01
 C24A-C22A = C23A-C22A = C21A-C20A
 1.52 with sigma of 0.01
 P4-C44 \\sim P5-C63 \\sim P4-C46 \\sim P5-C61
 with sigma of 0.02
 P2-C5 \\sim P2-C5A
 with sigma of 0.02
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 C5-C10 \\sim C5A-C10A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
 C9-C10 \\sim C9A-C10A
 with sigma of 0.02
 P2-C6 \\sim P2-C6A
 with sigma of 0.04
 P2-C10 \\sim P2-C10A
 with sigma of 0.04
 C5-C7 \\sim C5A-C7A
 with sigma of 0.04
 C5-C9 \\sim C5A-C9A
 with sigma of 0.04
 C6-C8 \\sim C6A-C8A
 with sigma of 0.04
 C6-C10 \\sim C6A-C10A
 with sigma of 0.04
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
 C8-C10 \\sim C8A-C10A
 with sigma of 0.04
 P1-C21A \\sim P1-C22A
 with sigma of 0.02
3. Rigid bond restraints
 P4, C46, C47, C48, C44, C45, C63, C62, P5, C65, C61, C64
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C63, P5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 P1, C20, C21, C22, C23, C24, C22A, C24A, C23A, C20A, C21A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C20, C21
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C29, C30, C31, C32, C33, C34, C50, C40, C51, C49, C52, C53
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C5, C6, C7, C8, C9, C10, C5A, C6A, C7A, C8A, C9A, C10A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C14, C54, C13, C12, C60, C58, C59, C16, C15, C55, C57, C56
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C17, C19A, C18A, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 C41, C42, C43
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
4. Uiso/Uaniso restraints and constraints
P4 \\sim C46 \\sim C47 \\sim C48 \\sim C44 \\sim C45 \\sim C63 \\sim C62 \\sim
P5 \\sim C65 \\sim C61 \\sim C64: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C63 \\sim P5: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C22A \\sim C24A \\sim C23A
\\sim C20A \\sim C21A \\sim P1: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C20 \\sim C21: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C50 \\sim C40 \\sim
C51 \\sim C49 \\sim C52 \\sim C53: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C5A \\sim C6A \\sim C7A
\\sim C8A \\sim C9A \\sim C10A: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C14 \\sim C16 \\sim C15 \\sim C54 \\sim C13 \\sim C60 \\sim C55 \\sim C57 \\sim
C58 \\sim C56 \\sim C59 \\sim C12: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C17 \\sim C19A \\sim C18 \\sim C18A \\sim C19: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C41 \\sim C42 \\sim C43: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
5. Others
 Sof(C50)=Sof(H50)=Sof(C40)=Sof(H40)=Sof(C51)=Sof(H51)=Sof(C49)=Sof(C52)=
 Sof(H52)=Sof(C53)=Sof(H53)=1-FVAR(1)
 Sof(C29)=Sof(C30)=Sof(H30)=Sof(C31)=Sof(H31)=Sof(C32)=Sof(H32)=Sof(C33)=
 Sof(H33)=Sof(C34)=Sof(H34)=FVAR(1)
 Sof(C5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=
 Sof(H9A)=Sof(C10A)=Sof(H10A)=1-FVAR(2)
 Sof(C5)=Sof(C6)=Sof(H6)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=Sof(H9)=
 Sof(C10)=Sof(H10)=FVAR(2)
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C39A)=Sof(H39A)=Sof(C11A)=
 Sof(H11A)=Sof(C36A)=Sof(H36A)=Sof(C35A)=1-FVAR(3)
 Sof(C35)=Sof(C36)=Sof(H36)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=
 Sof(H39)=Sof(C11)=Sof(H11)=FVAR(3)
 Sof(C60)=Sof(H60)=Sof(C55)=Sof(H55)=Sof(C57)=Sof(H57)=Sof(C58)=Sof(H58)=
 Sof(C56)=Sof(H56)=Sof(C59)=1-FVAR(4)
 Sof(C14)=Sof(H14)=Sof(C16)=Sof(H16)=Sof(C15)=Sof(H15)=Sof(C54)=Sof(H54)=
 Sof(C13)=Sof(H13)=Sof(C12)=FVAR(4)
 Sof(H17A)=Sof(C18)=Sof(H18D)=Sof(H18E)=Sof(H18F)=Sof(C19)=Sof(H19D)=Sof(H19E)=
 Sof(H19F)=1-FVAR(5)
 Sof(H17)=Sof(C18A)=Sof(H18A)=Sof(H18B)=Sof(H18C)=Sof(C19A)=Sof(H19A)=
 Sof(H19B)=Sof(H19C)=FVAR(5)
 Sof(C63)=Sof(H63)=Sof(C62)=Sof(H62A)=Sof(H62B)=Sof(H62C)=Sof(P5)=Sof(C65)=
 Sof(H65A)=Sof(H65B)=Sof(H65C)=Sof(C61)=Sof(H61A)=Sof(H61B)=Sof(C64)=Sof(H64A)=
 Sof(H64B)=Sof(H64C)=1-FVAR(6)
 Sof(P4)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C48)=
 Sof(H48A)=Sof(H48B)=Sof(H48C)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=
 Sof(H45B)=Sof(H45C)=FVAR(6)
 Sof(C22A)=Sof(H22A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C23A)=
 Sof(H23D)=Sof(H23E)=Sof(H23F)=Sof(C20A)=Sof(H20C)=Sof(H20D)=Sof(H20E)=
 Sof(C21A)=Sof(H21D)=Sof(H21E)=1-FVAR(7)
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=Sof(C22)=
 Sof(H22)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(C24)=Sof(H24A)=Sof(H24B)=
 Sof(H24C)=FVAR(7)
 Fixed X: C46(0.661631) C63(0.784829)
 Fixed Y: C63(0.38909)
 Fixed Z: C46(0.1427) C22(0.537399) C63(0.2278)
6.a Ternary CH refined with riding coordinates:
 C46(H46), C17(H17), C17(H17A), C22(H22), C41(H41), C63(H63), C22A(H22A)
6.b Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C44(H44A,H44B), C61(H61A,H61B), C21A(H21D,H21E)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C8(H8), C9(H9), C10(H10), C30(H30), C31(H31), C32(H32),
 C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C11(H11), C14(H14),
  C16(H16), C15(H15), C54(H54), C13(H13), C50(H50), C40(H40), C51(H51),
 C52(H52), C53(H53), C6A(H6A), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A),
 C37A(H37A), C38A(H38A), C39A(H39A), C11A(H11A), C36A(H36A), C60(H60), C55(H55),
  C57(H57), C58(H58), C56(H56)
6.d Fitted hexagon refined as free rotating group:
 C5(C6,C7,C8,C9,C10), C29(C30,C31,C32,C33,C34), C14(C16,C15,C54,C13,C12),
 C5A(C6A,C7A,C8A,C9A,C10A), C37A(C38A,C39A,C11A,C36A,C35A)
6.e Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C48(H48A,H48B,H48C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C45(H45A,
 H45B,H45C), C18A(H18A,H18B,H18C), C19A(H19A,H19B,H19C), C18(H18D,H18E,H18F),
 C19(H19D,H19E,H19F), C62(H62A,H62B,H62C), C65(H65A,H65B,H65C), C64(H64A,H64B,
 H64C), C24A(H24D,H24E,H24F), C23A(H23D,H23E,H23F), C20A(H20C,H20D,H20E)
;
_shelx_res_checksum              68114
_shelx_hkl_checksum              7610
_olex2_submission_special_instructions 'No special instructions were received'