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_7125163
_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 Mn O'
_chemical_formula_sum            'C52 H58 Mn O'
_chemical_formula_weight         753.92
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-08-22
_audit_creation_method
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Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
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_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                   18.67834(16)
_cell_length_b                   21.44845(18)
_cell_length_c                   21.13621(17)
_cell_measurement_reflns_used    8357
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      73.8600
_cell_measurement_theta_min      3.1350
_cell_volume                     8467.62(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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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)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
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_diffrn_ambient_environment      N~2~
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_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 10.3271
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_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details
;
  1 omega  -49.00   19.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000    0.0000 68

  2 omega  -38.00   18.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000  120.0000 56

  3 omega   -1.00   32.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -38.5000   37.0000   30.0000 33

  4 omega  -19.00   40.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       43.0073  -77.0000  150.0000 59

  5 omega   50.00   84.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000 -150.0000 34

  6 omega   31.00   64.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000    0.0000 33

  7 omega   20.00  157.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000    0.0000  -90.0000 137

  8 omega   41.00   94.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000 -180.0000 53

  9 omega   41.00   97.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  -60.0000 56

 10 omega   36.00   98.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -45.0000  120.0000 62

 11 omega   32.00   59.00   1.0000   16.0000
omega____ theta____ kappa____ phi______ frames
    -      104.5000  -30.0000  -90.0000 27
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'GV1000, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'MiTeGen micromount'
_diffrn_orient_matrix_UB_11      0.0594342000
_diffrn_orient_matrix_UB_12      -0.0049147000
_diffrn_orient_matrix_UB_13      -0.0502254000
_diffrn_orient_matrix_UB_21      0.0050713000
_diffrn_orient_matrix_UB_22      0.0716593000
_diffrn_orient_matrix_UB_23      -0.0024715000
_diffrn_orient_matrix_UB_31      0.0569529000
_diffrn_orient_matrix_UB_32      -0.0012297000
_diffrn_orient_matrix_UB_33      0.0527528000
_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  0.0184
_diffrn_reflns_av_unetI/netI     0.0146
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16280
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.265
_diffrn_reflns_theta_min         3.771
_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    2.798
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
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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)
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            'light brown'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
_exptl_crystal_F_000             3224
_exptl_crystal_recrystallization_method 'Recrystallised in Hexanes'
_exptl_crystal_size_max          0.2361
_exptl_crystal_size_mid          0.1696
_exptl_crystal_size_min          0.0756
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0301
_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^)+(0.0435P)^2^+5.5131P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0814
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3904
_reflns_number_total             4254
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc07243g2.cif
_cod_data_source_block           1
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               7125163
_nottingham_internal_coll_name   MNHRSC
_nottingham_internal_coll_number 13988
_nottingham_internal_coll_client HRS/DLK
_nottingham_internal_coll_type   custom
_nottingham_internal_coll_frame_method 'omega scans'
_nottingham_internal_coll_frame_time '4.0000, 16.0000'
_nottingham_internal_coll_frame_width 1.0000
_nottingham_internal_coll_user   pcxhrs
_nottingham_internal_coll_date   18/09/2014
_nottingham_internal_coll_location NOTTS
_nottingham_internal_coll_instrument 'GVA, PL13110002'
_nottingham_internal_process_date 18/09/2014
_nottingham_internal_process_user pcxhrs
_nottingham_internal_solution_date 18/9/2014
_nottingham_internal_solution_user pcxhrs
_nottingham_internal_refinement_date 18/9/2014
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_nottingham_internal_self_validation_user 16/10/2014
_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 Mn O'
_chemical_oxdiff_usercomment
'MNHRSC #13988 GVA-315 MOUNTED IN FOMBLIN FILM ON MICROMOUNT FOR HRS/DLK'
_reflns_odcompleteness_completeness 99.93
_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(H25C)=Sof(H25D)=Sof(C26B)=Sof(H26C)=Sof(H26D)=1-FVAR(1)
 Sof(H25A)=Sof(H25B)=Sof(C26A)=Sof(H26A)=Sof(H26B)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C25(H25C,H25D), C26A(H26A,H26B), C26B(H26C,H26D)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C17(H17), C20(H20)
3.c 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)
;
_shelx_res_checksum              57103
_olex2_exptl_crystal_mounting_method 'in fomblin film on a micromount'
_olex2_submission_special_instructions 'No special instructions were received'