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_7125166
_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         'C48 H50 Li2'
_chemical_formula_sum            'C48 H50 Li2'
_chemical_formula_weight         640.76
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-05-28
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;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_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                   12.4731(2)
_cell_length_b                   12.4731(2)
_cell_length_c                   48.7421(15)
_cell_measurement_reflns_used    11236
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      74.1730
_cell_measurement_theta_min      3.5910
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
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_diffrn_ambient_environment      'N2 gas'
_diffrn_ambient_temperature      120(2)
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_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3613
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_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -14.00   26.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   38.0000   30.0000 40

  2 omega -111.00  -33.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000  -38.0000 -150.0000 78

  3 omega   79.00  159.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087   61.0000  120.0000 80

  4 omega   39.00   91.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -45.0000  -90.0000 52

  5 omega   44.00   94.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -45.0000   90.0000 50

  6 omega   45.00   75.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -45.0000  150.0000 30

  7 omega   66.00   91.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  -30.0000 -150.0000 25

  8 omega   17.00  114.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   53.0000   80.0000 97

  9 omega   17.00  113.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       43.3152   57.0000  -30.0000 96

 10 omega   94.00  177.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  125.0000 -150.0000 83

 11 omega   94.00  142.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8087  125.0000   30.0000 48
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      0.0019126000
_diffrn_orient_matrix_UB_12      -0.0777049000
_diffrn_orient_matrix_UB_13      -0.0245591000
_diffrn_orient_matrix_UB_21      -0.1227662000
_diffrn_orient_matrix_UB_22      -0.0116908000
_diffrn_orient_matrix_UB_23      0.0017736000
_diffrn_orient_matrix_UB_31      -0.0134648000
_diffrn_orient_matrix_UB_32      0.0952739000
_diffrn_orient_matrix_UB_33      -0.0198126000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            31941
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.365
_diffrn_reflns_theta_min         3.658
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.460
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_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       block
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.1276
_exptl_crystal_size_min          0.0525
_refine_diff_density_max         0.134
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.029
_refine_ls_abs_structure_details
;
 Flack x determined using 2592 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     463
_refine_ls_number_reflns         7589
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_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0552P)^2^+0.1836P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.694
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.966
_reflns_number_gt                6878
_reflns_number_total             7589
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07243g2.cif
_cod_data_source_block           7
_cod_original_cell_volume        7583.3(4)
_cod_database_code               7125166
_nottingham_internal_coll_name   CHRSLC
_nottingham_internal_coll_number 13922
_nottingham_internal_coll_client HRS/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '30.0000, 120.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxhrs
_nottingham_internal_coll_date   21/08/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 22/08/2014
_nottingham_internal_process_user pcxhrs
_nottingham_internal_solution_date 28/05/2015
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_nottingham_internal_refinement_date 28/05/2015
_nottingham_internal_refinement_user pcxtb
_nottingham_internal_self_archive_date 28/05/2015
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_nottingham_internal_self_validation_user pcxtb
_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         'C48 H50 Li2'
_chemical_oxdiff_usercomment
'CHRSLC #13922 MOUNTED ON A MICROMOUNT IN FOMBLIN FILM FOR HRS/DLK'
_reflns_odcompleteness_completeness 99.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C17(H17), C20(H20), C27(H27),
 C28(H28), C29(H29), C32(H32), C35(H35), C41(H41), C44(H44)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C), C39(H39A,H39B,H39C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C)
;
_shelx_res_checksum              99176
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'