Synthesis and characterization of manganese triple-decker complexes.
Heinl, Sebastian; Balázs, Gábor; Bodensteiner, Michael; Scheer, Manfred; Dalton transactions (Cambridge, England : 2003) 45 (2016) 1962–1966; doi:10.1039/c5dt01750e

data_7035321
_publ_section_title
;
 Synthesis and characterization of manganese triple-decker complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1962
_journal_page_last               1966
_journal_paper_doi               10.1039/c5dt01750e
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C62 H73 Mn'
_chemical_formula_sum            'C62 H73 Mn'
_chemical_formula_weight         873.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.19 svn.r3143 for OlexSys, GUI svn.r4992)
;
_audit_update_record
;
2015-02-09 deposited with the CCDC.
2015-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                105.957(3)
_cell_angle_beta                 94.745(3)
_cell_angle_gamma                118.726(4)
_cell_formula_units_Z            2
_cell_length_a                   14.1067(7)
_cell_length_b                   14.5710(5)
_cell_length_c                   14.6081(5)
_cell_measurement_reflns_used    9013
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      70.8852
_cell_measurement_theta_min      3.2540
_cell_volume                     2448.1(2)
_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
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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_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3546
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_details
;
  1 omega -116.00  -16.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -37.0000 -120.0000 100

  2 omega  -67.00   32.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064   37.0000   60.0000 99

  3 omega    3.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064 -125.0000 -180.0000 95

  4 omega   34.00  123.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429 -127.0000   41.0000 89

  5 omega   74.00  158.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   45.0000   90.0000 84

  6 omega   30.00   77.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -45.0000  120.0000 47

  7 omega   69.00  109.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -94.0000  150.0000 40

  8 omega   19.00   47.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -94.0000  150.0000 28

  9 omega   19.00  158.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429    0.0000 -120.0000 139

 10 omega   23.00  135.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -77.0000 -150.0000 112

 11 omega   23.00   69.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -30.0000 -150.0000 46

 12 omega   22.00  135.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -77.0000   30.0000 113

 13 omega -115.00  -12.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000  150.0000 103

 14 omega    8.00  120.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   77.0000   30.0000 112

 15 omega    2.00   98.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064 -125.0000  -60.0000 96

 16 omega   74.00  107.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   45.0000   30.0000 33

 17 omega   23.00   69.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429  -30.0000   30.0000 46

 18 omega   71.00  140.00   1.0000  140.0000
omega____ theta____ kappa____ phi______ frames
    -      101.1429   30.0000  -30.0000 69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1162114000
_diffrn_orient_matrix_UB_12      -0.0146008000
_diffrn_orient_matrix_UB_13      -0.0212383000
_diffrn_orient_matrix_UB_21      -0.0145927000
_diffrn_orient_matrix_UB_22      -0.0519384000
_diffrn_orient_matrix_UB_23      -0.1112121000
_diffrn_orient_matrix_UB_31      -0.0535528000
_diffrn_orient_matrix_UB_32      -0.1174350000
_diffrn_orient_matrix_UB_33      0.0068786000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_laue_measured_fraction_full 0.990
_diffrn_reflns_laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20568
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.000
_diffrn_reflns_theta_max         70.879
_diffrn_reflns_theta_min         3.254
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.469
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.780
_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 dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_description       plate
_exptl_crystal_F_000             940
_exptl_crystal_size_max          0.162
_exptl_crystal_size_mid          0.0788
_exptl_crystal_size_min          0.0243
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         9066
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0623P)^2^+0.8722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1163
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8049
_reflns_number_total             9066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt01750e2.cif
_cod_data_source_block           sh357
_cod_depositor_comments
'Adding full bibliography for 7035321--7035322.cif.'
_cod_original_cell_volume        2448.09(19)
_cod_database_code               7035321
_shelxl_version_number           2014/6
_chemical_oxdiff_formula         C62H73Mn
_reflns_odcompleteness_completeness 98.95
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C57A \\sim C57: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.02
3. Others
 Fixed Sof: C56(0.78) H56A(0.78) H56B(0.78) C57(0.78) H57(0.78) H58(0.78)
 H58A(0.22) H62(0.78) H62A(0.22) C57A(0.22) H57A(0.22) C56A(0.22) H56C(0.22)
 H56D(0.22)
4.a Ternary CH refined with riding coordinates:
 C57(H57), C58(H58), C58(H58A), C62(H62), C62(H62A), C57A(H57A)
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C22(H22A,H22B), C23(H23A,
 H23B), C24(H24A,H24B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B),
 C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B), C56(H56A,H56B), C56A(H56C,H56D)
4.c Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C), C45(H45A,H45B,
 H45C), C55(H55A,H55B,H55C)
4.d Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C17(H17), C18(H18), C19(H19), C20(H20),
 C27(H27), C28(H28), C29(H29), C30(H30), C37(H37), C38(H38), C39(H39), C40(H40),
  C47(H47), C48(H48), C49(H49), C50(H50), C59(H59), C60(H60), C61(H61)
;
_olex2_submission_special_instructions 'No special instructions were received'