Cycloheptyl-fused N,N,N'-chromium catalysts with selectivity for vinyl-terminated polyethylene waxes: thermal optimization and polymer functionalization.
Huang, Chuanbing; Huang, Yongfeng; Ma, Yanping; Solan, Gregory A.; Sun, Yang; Hu, Xinquan; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 47 (2018) 13487–13497; doi:10.1039/c8dt03052a

data_7047400
_publ_section_title
;
 Cycloheptyl-fused N,N,N'-chromium catalysts with selectivity for
 vinyl-terminated polyethylene waxes: thermal optimization and polymer
 functionalization.
;
_journal_issue                   38
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13487
_journal_page_last               13497
_journal_paper_doi               10.1039/c8dt03052a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C32 H39 Cl3 Cr N3'
_chemical_formula_sum            'C32 H39 Cl3 Cr N3'
_chemical_formula_weight         624.01
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-02-08
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_audit_update_record
;
2018-07-26 deposited with the CCDC.
2018-08-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.413(3)
_cell_length_b                   15.526(3)
_cell_length_c                   15.772(3)
_cell_measurement_reflns_used    10248
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4854
_cell_measurement_theta_min      1.2911
_cell_volume                     3039.6(11)
_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  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 99.7000
_diffrn_measured_fraction_theta_max 27.4854
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9172
              2theta: -20.2333
scan:
    Number of images: 270
               Slice: -76.2500 - 58.7500
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9172
              2theta: -20.2333
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0629
_diffrn_orient_matrix_UB_12      -0.0498
_diffrn_orient_matrix_UB_13      -0.0070
_diffrn_orient_matrix_UB_21      -0.0300
_diffrn_orient_matrix_UB_22      0.0432
_diffrn_orient_matrix_UB_23      -0.0372
_diffrn_orient_matrix_UB_31      0.0264
_diffrn_orient_matrix_UB_32      -0.0260
_diffrn_orient_matrix_UB_33      -0.0514
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.710747
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20814
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_min         1.841
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8093
_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    1.364
_exptl_crystal_description       plate
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.553
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.085
_refine_ls_abs_structure_details
;
 Flack x determined using 2694 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.007(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0702P)^2^+2.0653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1256
_reflns_Friedel_coverage         0.785
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                6733
_reflns_number_total             6922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03052a2.cif
_cod_data_source_block           Cr2
_cod_depositor_comments          'Adding full bibliography for 7047400.cif.'
_cod_original_cell_volume        3039.5(11)
_cod_database_code               7047400
_diffrn_number_total             3905
_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.a Secondary CH2 refined with riding coordinates:
 C31(H17A,H17B), C14(H23A,H23B), C24(H25A,H25B), C21(H26A,H26B), C11(H3A,H3B),
 C10(H7A,H7B), C9(H8A,H8B), C12(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 C28(H9AA), C16(H2AA), C26(H5AA), C4(H16), C18(H18), C17(H20), C5(H22), C27(H32)
2.c Idealised Me refined as rotating group:
 C1(H27A,H27B,H27C), C23(H35A,H35B,H35C), C13(H54A,H54B,H54C), C32(H56A,H56B,
 H56C), C22(H1A,H1B,H1C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'