Cyclotrimerisation of isocyanates catalysed by low-coordinate Mn(ii) and Fe(ii) m-terphenyl complexes.
Sharpe, Helen R.; Geer, Ana M.; Williams, Huw E. L.; Blundell, Toby J.; Lewis, William; Blake, Alexander J.; Kays, Deborah L.; Chemical communications (Cambridge, England) 53 (2017) 937–940; doi:10.1039/c6cc07243g

data_7125164
_publ_section_title
;
 Cyclotrimerisation of isocyanates catalysed by low-coordinate Mn(ii) and
 Fe(ii) m-terphenyl complexes.
;
_journal_issue                   5
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              937
_journal_page_last               940
_journal_paper_doi               10.1039/c6cc07243g
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C52 H58 Fe O'
_chemical_formula_sum            'C52 H58 Fe O'
_chemical_formula_weight         754.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-08-24 deposited with the CCDC.
2016-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.6528(2)
_cell_length_b                   43.7692(5)
_cell_length_c                   10.50646(11)
_cell_measurement_reflns_used    18511
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.0310
_cell_measurement_theta_min      4.3060
_cell_volume                     8577.66(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.6296
_diffrn_detector_type            'Agilent Diffraction Atlas detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega    7.00   33.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   60.0000 26

  2 omega  -59.00  -17.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000  -30.0000 42

  3 omega  -35.00   -2.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  125.0000 -180.0000 33

  4 omega  -47.00   30.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000  -60.0000 77

  5 omega   31.00   87.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  120.0000 56

  6 omega   52.00   86.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000    0.0000 34

  7 omega   92.00  174.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   45.0000 -120.0000 82

  8 omega   32.00   83.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -60.0000 51

  9 omega   33.00   69.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -90.0000 36

 10 omega  123.00  158.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   61.0000   90.0000 35

 11 omega    2.00   95.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4304 -125.0000 -150.0000 93

 12 omega   13.00  111.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4304   72.0000  -33.0000 98

 13 omega   16.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4304   57.0000 -180.0000 94

 14 omega   73.00  163.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  125.0000  -90.0000 90

 15 omega   84.00  178.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000   30.0000   60.0000 94

 16 omega   25.00  109.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -94.0000  -90.0000 84
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0629048000
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_diffrn_orient_matrix_UB_13      -0.0934427000
_diffrn_orient_matrix_UB_21      -0.0258350000
_diffrn_orient_matrix_UB_22      0.0280165000
_diffrn_orient_matrix_UB_23      0.0759867000
_diffrn_orient_matrix_UB_31      0.0468622000
_diffrn_orient_matrix_UB_32      0.0209081000
_diffrn_orient_matrix_UB_33      -0.0836610000
_diffrn_radiation_collimation    'focusing mirrors'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_wavelength_determination fundamental
_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            50578
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.211
_diffrn_reflns_theta_min         4.040
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_target            Cu
_diffrn_source_type              'Agilent Diffraction microfocus tube'
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    3.079
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_description       block
_exptl_crystal_F_000             3232
_exptl_crystal_recrystallization_method 'Recrystallised in Hexanes'
_exptl_crystal_size_max          0.2723
_exptl_crystal_size_mid          0.1438
_exptl_crystal_size_min          0.0917
_refine_diff_density_max         0.444
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         8631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0334P)^2^+8.4968P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1067
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7751
_reflns_number_total             8631
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07243g2.cif
_cod_data_source_block           2
_cod_original_cell_volume        8577.65(17)
_cod_database_code               7125164
_nottingham_internal_coll_name   FEHRSI
_nottingham_internal_coll_number 13763
_nottingham_internal_coll_client HRS/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '25.0000, 100.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxhrs
_nottingham_internal_coll_date   02/07/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 03/07/2014
_nottingham_internal_process_user pcxhrs
_nottingham_internal_solution_date 03/07/2014
_nottingham_internal_solution_user pcxhrs
_nottingham_internal_refinement_date 18/09/2014
_nottingham_internal_refinement_user pcxhrs
_nottingham_internal_self_archive_date 18/09/2014
_nottingham_internal_self_validation_date 18/09/2014
_nottingham_internal_self_validation_user pcxhrs
_nottingham_internal_validation_date 22/8/2016
_nottingham_internal_validation_user pczwl
_nottingham_internal_archive_date 22/8/2016
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C52 H58 Fe O'
_chemical_oxdiff_usercomment
'FEHRSI #13763 GVB - 212 in fomblin film on micromount for HRS/DLK'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Others
 Sof(H52C)=Sof(H52D)=Sof(H49C)=Sof(H49D)=Sof(C51B)=Sof(H51A)=Sof(H51B)=
 Sof(C50B)=Sof(H50C)=Sof(H50D)=1-FVAR(1)
 Sof(H52A)=Sof(H52B)=Sof(H49A)=Sof(H49B)=Sof(C50A)=Sof(H50A)=Sof(H50B)=
 Sof(C51A)=Sof(H51C)=Sof(H51D)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C52(H52C,H52D), C52(H52A,H52B), C49(H49A,H49B), C49(H49C,H49D), C50A(H50A,
 H50B), C51B(H51A,H51B), C50B(H50C,H50D), C51A(H51C,H51D)
3.b Aromatic/amide H refined with riding coordinates:
 C44(H44), C41(H41), C8(H8), C32(H32), C29(H29), C20(H20), C35(H35), C28(H28),
 C17(H17), C27(H27), C11(H11), C3(H3), C5(H5), C4(H4)
3.c Idealised Me refined as rotating group:
 C38(H38A,H38B,H38C), C48(H48A,H48B,H48C), C22(H22A,H22B,H22C), C14(H14A,H14B,
 H14C), C37(H37A,H37B,H37C), C24(H24A,H24B,H24C), C13(H13A,H13B,H13C), C15(H15A,
 H15B,H15C), C39(H39A,H39B,H39C), C23(H23A,H23B,H23C), C47(H47A,H47B,H47C),
 C46(H46A,H46B,H46C)
;
_shelx_res_checksum              93461
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'