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_7702277
_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         'C42 H55 Cl2 Fe N3'
_chemical_formula_sum            'C42 H55 Cl2 Fe N3'
_chemical_formula_weight         728.64
_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     iterative
_audit_creation_date             2018-12-10
_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                 118.227(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5657(15)
_cell_length_b                   16.2635(16)
_cell_length_c                   17.7642(17)
_cell_measurement_reflns_used    3918
_cell_measurement_temperature    170.00(10)
_cell_measurement_theta_max      21.5040
_cell_measurement_theta_min      3.5650
_cell_volume                     4471.4(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45i (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45i (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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    -47.00 -20.00   0.50   15.00    --  -15.00  45.00  60.00   54
  2  \w   -100.00 -53.00   0.50   15.00    --  -15.00  45.00 150.00   94
  3  \w     30.00  57.00   0.50   15.00    --  -15.00  45.00 150.00   54
  4  \w    -91.00 -14.00   0.50   15.00    --  -15.00  45.00  90.00  154
  5  \w     37.00  62.00   0.50   15.00    --  -15.00  45.00  90.00   50
  6  \w   -103.00  74.00   0.50   15.00    --  -15.00  45.00   0.00  354
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC10 (RCD3): fixed-chi single'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.1190
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38773
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         3.415
_exptl_absorpt_coefficient_mu    0.485
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.37451
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45i (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    1.082
_exptl_crystal_description       rod
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.907
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         10242
_refine_ls_number_restraints     317
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.1910
_refine_ls_R_factor_gt           0.0950
_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^)+(0.1768P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2562
_refine_ls_wR_factor_ref         0.3130
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4448
_reflns_number_total             10242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt04325j1.cif
_cod_data_source_block           Fe3
_cod_depositor_comments
'Adding full bibliography for 7702277--7702278.cif.'
_cod_original_cell_volume        4471.4(8)
_cod_database_code               7702277
_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
 C22-C21 = C23-C22 = C24-C23 = C25-C24 = C26-C25 = C27-C26 = C27-C20
 1.54 with sigma of 0.01
 C27-C20 = C27-C41A = C41A-C40A = C40A-C39A = C39A-C38A = C38A-C37A = C37A-C21
 1.54 with sigma of 0.01
 C38-C37 = C36-C37
 1.54 with sigma of 0.01
 C42-C14A = C42-C41 = C14A-C13A = C13A-C12A = C12A-C38 = C41-C40 = C40-C39 =
 C39-C38
 1.54 with sigma of 0.01
 C40A-C38A
 2.5 with sigma of 0.02
 C27-C40A
 2.5 with sigma of 0.02
 C39A-C41A
 2.5 with sigma of 0.02
3. Rigid bond restraints
 C4, C5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C6, C7
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C22 \\sim C23 \\sim C24 \\sim C25 \\sim C26 \\sim C27 \\sim C41A \\sim C40A
\\sim C39A \\sim C38A \\sim C37A: within 1.7A with sigma of 0.02 and sigma for
terminal atoms of 0.04
H37a \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C14A \\sim C13A
\\sim C12A \\sim C37: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(C22) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C25)
\\sim Ueq, Uanis(C26) \\sim Ueq, Uanis(C27) \\sim Ueq, Uanis(C41A) \\sim Ueq,
Uanis(C40A) \\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C38A) \\sim Ueq,
Uanis(C37A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C40) \\sim Ueq, Uanis(C41)
\\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C12A) \\sim Ueq:
with sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(H38c)=Sof(H38d)=Sof(H42c)=Sof(H42d)=Sof(C14A)=Sof(H14a)=Sof(H14b)=
 Sof(C13A)=Sof(H13a)=Sof(H13b)=Sof(C12A)=Sof(H12a)=Sof(H12b)=1-FVAR(1)
 Sof(H38a)=Sof(H38b)=Sof(C39)=Sof(H39a)=Sof(H39b)=Sof(C40)=Sof(H40a)=Sof(H40b)=
 Sof(C41)=Sof(H41a)=Sof(H41b)=Sof(H42a)=Sof(H42b)=FVAR(1)
 Sof(H21c)=Sof(H21d)=Sof(H27c)=Sof(H27d)=Sof(C41A)=Sof(H41c)=Sof(H41d)=
 Sof(C40A)=Sof(H40c)=Sof(H40d)=Sof(C39A)=Sof(H39c)=Sof(H39d)=Sof(C38A)=
 Sof(H38e)=Sof(H38f)=Sof(C37A)=Sof(H37c)=Sof(H37d)=1-FVAR(2)
 Sof(H21a)=Sof(H21b)=Sof(C22)=Sof(H22a)=Sof(H22b)=Sof(C23)=Sof(H23a)=Sof(H23b)=
 Sof(C24)=Sof(H24a)=Sof(H24b)=Sof(C25)=Sof(H25a)=Sof(H25b)=Sof(C26)=Sof(H26a)=
 Sof(H26b)=Sof(H27a)=Sof(H27b)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C35(H35), C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C36(H36a,H36b), C37(H37a,H37b), C38(H38a,H38b), C38(H38c,H38d), C39(H39a,
 H39b), C40(H40a,H40b), C41(H41a,H41b), C42(H42a,H42b), C42(H42c,H42d),
 C10(H10a,H10b), C9(H9a,H9b), C8(H8a,H8b), C7(H7a,H7b), C21(H21a,H21b),
 C21(H21c,H21d), C22(H22a,H22b), C23(H23a,H23b), C24(H24a,H24b), C25(H25a,H25b),
  C26(H26a,H26b), C27(H27a,H27b), C27(H27c,H27d), C14A(H14a,H14b), C13A(H13a,
 H13b), C12A(H12a,H12b), C41A(H41c,H41d), C40A(H40c,H40d), C39A(H39c,H39d),
 C38A(H38e,H38f), C37A(H37c,H37d)
6.c Aromatic/amide H refined with riding coordinates:
 C30(H30), C31(H31), C32(H32), C4(H4), C5(H5), C15(H15), C16(H16), C17(H17)
6.d Idealised Me refined as rotating group:
 C34(H34a,H34b,H34c), C1(H1a,H1b,H1c), C19(H19a,H19b,H19c)
;
_shelx_res_checksum              90079
_shelx_fab_checksum              97115
_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
;