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_7125165
_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         'C24 H25 I'
_chemical_formula_sum            'C24 H25 I'
_chemical_formula_weight         440.34
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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Olex2 1.2
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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            4
_cell_length_a                   5.8071(4)
_cell_length_b                   27.443(2)
_cell_length_c                   12.2554(8)
_cell_measurement_reflns_used    2098
_cell_measurement_temperature    120(2)
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_cell_measurement_theta_min      3.9150
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_environment      N~2~
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_diffrn_measurement_details
;
  1 omega   24.00  112.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       43.6627   57.0000  150.0000 88

  2 omega  -25.00    3.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       43.6627  -57.0000    0.0000 28

  3 omega   37.00   68.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       43.6627  -57.0000    0.0000 31

  4 omega   36.00   63.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000   60.0000 27

  5 omega   71.00  102.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000 -150.0000 31

  6 omega   36.00   74.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -180.0000 38

  7 omega   51.00  106.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000   60.0000 55

  8 omega   33.00   58.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  -30.0000 25

  9 omega   42.00   70.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -45.0000 -150.0000 28

 10 omega   27.00   56.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -95.0000 -150.0000 29

 11 omega   36.00   69.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  -60.0000 33

 12 omega   38.00   67.00   1.0000   24.0000
omega____ theta____ kappa____ phi______ frames
    -      105.8472  -30.0000  -90.0000 29
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
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_diffrn_orient_matrix_UB_11      -0.0434744000
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_diffrn_orient_matrix_UB_13      0.0211974000
_diffrn_orient_matrix_UB_21      0.2490371000
_diffrn_orient_matrix_UB_22      0.0116681000
_diffrn_orient_matrix_UB_23      -0.0346390000
_diffrn_orient_matrix_UB_31      -0.0801947000
_diffrn_orient_matrix_UB_32      0.0063947000
_diffrn_orient_matrix_UB_33      -0.1189644000
_diffrn_radiation_monochromator  mirror
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_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4826
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
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_diffrn_reflns_theta_min         3.950
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.877
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_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Numerical absorption correction based on gaussian integration over
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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    1.498
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.132
_exptl_crystal_size_mid          0.1178
_exptl_crystal_size_min          0.0228
_refine_diff_density_max         2.650
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         1976
_refine_ls_number_restraints     0
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_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0472P)^2^+13.3354P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1220
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1754
_reflns_number_total             1976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07243g2.cif
_cod_data_source_block           6
_cod_original_cell_volume        1953.1(3)
_cod_database_code               7125165
_nottingham_internal_coll_name   OTBALC
_nottingham_internal_coll_number 12257
_nottingham_internal_coll_client TB/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '6.0000, 24.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxtb
_nottingham_internal_coll_date   23/02/2013
_nottingham_internal_coll_location NOTTS
_nottingham_internal_process_date 01/08/2014
_nottingham_internal_process_user pcxtb
_nottingham_internal_solution_date 28/05/2015
_nottingham_internal_solution_user pcxtb
_nottingham_internal_refinement_date 28/05/2015
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_nottingham_internal_validation_user pczwl
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_chemical_oxdiff_formula         'C24 H25 I'
_chemical_oxdiff_usercomment
'OTBALC #12257 MOUNTED IN FOMBLIN FILM ON MICROMOUNT FOR TB/DLK'
_reflns_odcompleteness_completeness 99.86
_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), C7(H7), C10(H10)
2.b Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              92613
_olex2_exptl_crystal_mounting_method "'in fomblin film on a micromount"
_olex2_submission_special_instructions 'No special instructions were received'