Probing the effect of ortho-cycloalkyl ring size on activity and thermostability in cycloheptyl-fused N,N,N-iron ethylene polymerization catalysts.
Guo, Jingjing; Zhang, Wenjuan; Oleynik, Ivan I.; Solan, Gregory A.; Oleynik, Irina V.; Liang, Tongling; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 49 (2020) 136–146; doi:10.1039/c9dt04325j

data_7702278
_publ_section_title
;
 Probing the effect of ortho-cycloalkyl ring size on activity and
 thermostability in cycloheptyl-fused N,N,N-iron ethylene polymerization
 catalysts.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              136
_journal_page_last               146
_journal_paper_doi               10.1039/c9dt04325j
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C44 H59 Cl2 Fe N3'
_chemical_formula_sum            'C44 H59 Cl2 Fe N3'
_chemical_formula_weight         756.69
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-28
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2019-09-15 deposited with the CCDC.	2019-11-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.961(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.004(2)
_cell_length_b                   16.1859(11)
_cell_length_c                   18.7893(14)
_cell_measurement_reflns_used    2168
_cell_measurement_temperature    169.99(12)
_cell_measurement_theta_max      65.2740
_cell_measurement_theta_min      3.6690
_cell_volume                     3977.1(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.14e (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      170
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -66.00  14.00   0.50    4.00    --  -47.20  93.00 103.00  160
  2  \w    -91.00 -65.00   0.50    8.00    --  -99.00  93.00 103.00   52
  3  \w   -114.00 -71.00   0.50    8.00    --  -99.00  61.00 150.00   86
  4  \w   -166.00 -86.00   0.50    8.00    --  -99.00 -30.00  60.00  160
  5  \w   -101.00 -76.00   0.50    4.00    --  -47.20-125.00 150.00   50
  6  \w   -116.00 -83.00   0.50    4.00    --  -47.20-125.00  60.00   66
  7  \w    -18.00  56.00   0.50    4.00    --   47.20 -93.00  -8.00  148
  8  \w     32.00 108.00   0.50    8.00    --  103.25 -93.00  -8.00  152
  9  \w     54.00 116.00   0.50    8.00    --  103.25 -45.00   0.00  124
 10  \w     75.00 107.00   0.50    8.00    --  103.25 -30.00 -30.00   64
 11  \w     99.00 164.00   0.50    8.00    --  103.25  45.00  30.00  130
 12  \w    117.00 143.00   0.50    8.00    --  103.25  93.00 103.00   52
 13  \w     87.00 114.00   0.50    8.00    --  103.25  93.00 103.00   54
 14  \w     85.00 156.00   0.50    8.00    --  103.25  77.00 150.00  142
 15  \w     30.00  71.00   0.50    8.00    --  103.25 -30.00 -30.00   82
 16  \w    -26.00  44.00   0.50    4.00    --   47.20 -38.00-120.00  140
 17  \w   -125.00 -88.00   0.50    8.00    --  -99.00 -30.00-180.00   74
 18  \w   -167.00-141.00   0.50    8.00    --  -99.00 -30.00-180.00   52
 19  \w   -168.00 -84.00   0.50    8.00    --  -99.00 -93.00  -8.00  168
 20  \w   -168.00 -91.00   0.50    8.00    --  -99.00 -45.00  30.00  154
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1483
_diffrn_reflns_av_unetI/netI     0.1020
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30686
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.821
_diffrn_reflns_theta_min         3.380
_exptl_absorpt_coefficient_mu    4.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.14e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             1616
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         7942
_refine_ls_number_restraints     435
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.2279
_refine_ls_R_factor_gt           0.0895
_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^)+(0.1552P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2360
_refine_ls_wR_factor_ref         0.3247
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2535
_reflns_number_total             7942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04325j1.cif
_cod_data_source_block           Fe6
_cod_depositor_comments
'Adding full bibliography for 7702277--7702278.cif.'
_cod_database_code               7702278
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C16-C15 = C17-C16 = C18-C17 = C19-C18 = C20-C19 = C21-C20 = C22-C21
 1.54 with sigma of 0.01
 C16A-C15 = C17A-C16A = C18A-C17A = C19A-C18A = C20A-C19A = C21A-C20A = C22-
 C21A = C22-C15
 1.54 with sigma of 0.01
 C33-C32 = C33-C01B = C34-C01B = C35-C34 = C36-C35
 1.54 with sigma of 0.01
 C31A-C30 = C32A-C31A = C33-C32A = C33-C01C = C34-C01C = C35-C34
 1.54 with sigma of 0.01
 C36-C31A
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C22 \\sim C15 \\sim C16 \\sim C20A \\sim C18 \\sim C17 \\sim C21 \\sim C19
\\sim C20 \\sim C19A \\sim C21A \\sim C18A \\sim C17A \\sim C16A: within 1.7A
with sigma of 0.02 and sigma for terminal atoms of 0.04
C30 \\sim C36 \\sim C31A \\sim C33 \\sim C35 \\sim C01B \\sim C34 \\sim C32
\\sim C01C \\sim C31 \\sim C32A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C22) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C20A)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C21) \\sim Ueq,
Uanis(C19) \\sim Ueq, Uanis(C20) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C21A)
\\sim Ueq, Uanis(C18A) \\sim Ueq, Uanis(C17A) \\sim Ueq, Uanis(C16A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C33) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(C01B) \\sim Ueq, Uanis(C34) \\sim Ueq, Uanis(C32) \\sim Ueq,
Uanis(C01C) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C32A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(H33C)=Sof(H33D)=Sof(H34C)=Sof(H34D)=Sof(C01C)=Sof(H01C)=Sof(H01D)=1-FVAR(1)
 Sof(H33A)=Sof(H33B)=Sof(C01B)=Sof(H01A)=Sof(H01B)=Sof(H34A)=Sof(H34B)=FVAR(1)
 Sof(C20A)=Sof(H20A)=Sof(H20B)=1-FVAR(2)
 Sof(C20)=Sof(H20C)=Sof(H20D)=FVAR(2)
 Sof(H30A)=Sof(C31A)=Sof(H31A)=Sof(H31B)=1-FVAR(3)
 Sof(H30)=Sof(C31)=Sof(H31C)=Sof(H31D)=FVAR(3)
 Sof(C19A)=Sof(H19C)=Sof(H19D)=1-FVAR(4)
 Sof(C19)=Sof(H19A)=Sof(H19B)=FVAR(4)
 Sof(H22C)=Sof(H22D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=1-FVAR(5)
 Sof(H22A)=Sof(H22B)=Sof(C21)=Sof(H21A)=Sof(H21B)=FVAR(5)
 Sof(H15A)=Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C17A)=Sof(H17C)=Sof(H17D)=
 Sof(C16A)=Sof(H16C)=Sof(H16D)=1-FVAR(6)
 Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C17)=
 Sof(H17A)=Sof(H17B)=FVAR(6)
 Sof(C32A)=Sof(H32C)=Sof(H32D)=1-FVAR(7)
 Sof(C32)=Sof(H32A)=Sof(H32B)=FVAR(7)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C15(H15A), C30(H30A), C30(H30)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C22(H22C,H22D), C10(H10A,H10B), C8(H8A,H8B), C7(H7A,H7B),
 C9(H9A,H9B), C16(H16A,H16B), C20A(H20A,H20B), C18(H18A,H18B), C36(H36A,H36B),
 C31A(H31A,H31B), C17(H17A,H17B), C21(H21A,H21B), C33(H33A,H33B), C33(H33C,
 H33D), C35(H35A,H35B), C01B(H01A,H01B), C19(H19A,H19B), C34(H34A,H34B),
 C34(H34C,H34D), C32(H32A,H32B), C01C(H01C,H01D), C20(H20C,H20D), C31(H31C,
 H31D), C19A(H19C,H19D), C21A(H21C,H21D), C18A(H18C,H18D), C17A(H17C,H17D),
 C16A(H16C,H16D), C32A(H32C,H32D)
5.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C23(H23), C5(H5), C4(H4), C39(H39), C37(H37)
5.d Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C41(H41A,H41B,H41C), C1(H1A,H1B,H1C), C43(H43A,H43B,
 H43C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              54084
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;