Single- and double-bridged PNP ligands in chromium-catalysed ethylene oligomerisation
Lo, Quintin; Pye, Dominic; Gesslbauer, Sami; Sim, Ying; García, Felipe; White, Andrew J. P.; Britovsek, George J. P.; Catalysis Science & Technology 12 (2022) 4544–4551; doi:10.1039/D2CY00550F

data_1567086
_publ_section_title
;
 Single- and double-bridged PNP ligands in chromium-catalysed ethylene
 oligomerisation
;
_journal_issue                   14
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              4544
_journal_page_last               4551
_journal_paper_doi               10.1039/D2CY00550F
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C22 H54 Cl6 Cr2 N10 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C24 H58 Cl10 Cr2 N10 P4'
_chemical_formula_weight         1069.18
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-07 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.406(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3625(3)
_cell_length_b                   12.7925(3)
_cell_length_c                   19.2108(5)
_cell_measurement_reflns_used    3347
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0330
_cell_measurement_theta_min      2.9630
_cell_volume                     2286.51(11)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.810
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8211
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_min         2.662
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'Dark blue'
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1100
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     284
_refine_ls_number_reflns         4609
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0359P)^2^+4.4395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3857
_reflns_number_total             4609
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cy00550f2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1567084--1567086.cif.'
_cod_original_cell_volume        2286.52(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1567086
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              47053