2-Benzimidazol-6-pyrazol-pyridine Chromium(III) Trichlorides: Synthesis, Characterization, and Application for Ethylene Oligomerization and Polymerization
Luo, Wenlong; Li, Antai; Liu, Shaofeng; Ye, Hongqi; Li, Zhibo; Organometallics 35 (2016) 3045–; doi:10.1021/acs.organomet.6b00573

data_4088944
_publ_section_title
;
 2-Benzimidazol-6-pyrazol-pyridine Chromium(III) Trichlorides: Synthesis,
 Characterization, and Application for Ethylene Oligomerization and
 Polymerization
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3045
_journal_paper_doi               10.1021/acs.organomet.6b00573
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C17 H15 Cl3 Cr N5, 2(C3 H7 N O)'
_chemical_formula_sum            'C23 H29 Cl3 Cr N7 O2'
_chemical_formula_weight         593.88
_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_date             2015-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 101.636(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.127(3)
_cell_length_b                   19.795(6)
_cell_length_c                   17.268(5)
_cell_measurement_reflns_used    9306
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4808
_cell_measurement_theta_min      1.2040
_cell_volume                     2720.9(15)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution
;
'SHELXT (Sheldrick, 2014)'
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
scan:
	Number of images: 360
	           Slice: -110.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 9.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 270.0000
	             XTD: 44.9962
	          2theta: -20.2132
scan:
	Number of images: 300
	           Slice: -80.0000 - 70.0000
	     Image width: 0.5000
	        Exp time: 9.0000
	   Rotation axis: Omega
	           Omega: 0.0000
	             Chi: 45.0000
	             Phi: 180.0000
	             XTD: 44.9962
	          2theta: -20.2132
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'MM007-HF CCD(Saturn 724+)'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0848
_diffrn_orient_matrix_UB_12      0.0720
_diffrn_orient_matrix_UB_13      -0.0584
_diffrn_orient_matrix_UB_21      0.0087
_diffrn_orient_matrix_UB_22      0.0371
_diffrn_orient_matrix_UB_23      0.0331
_diffrn_orient_matrix_UB_31      0.0335
_diffrn_orient_matrix_UB_32      0.0279
_diffrn_orient_matrix_UB_33      -0.0400
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_unetI/netI     0.0672
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20363
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.584
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2007)'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.450
_exptl_crystal_description       rod
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.274
_exptl_crystal_size_mid          0.081
_exptl_crystal_size_min          0.065
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0639
_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^)+(0.0465P)^2^+2.5433P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1430
_refine_ls_wR_factor_ref         0.1500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5436
_reflns_number_total             6255
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00573_si_002.cif
_cod_data_source_block           mx4378
_cod_original_cell_volume        2721.0(14)
_cod_database_code               4088944
_diffrn_number_total             6450
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), C2(H2), C7(H7), C8(H8), C9(H9), C13(H13), C14(H14), C15(H15),
 C16(H16), C20(H20), C23(H23)
2.b Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              20652
_shelx_hkl_checksum              49196
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'