The synthesis of the heterocubane cluster [{CpMn}4(mu3-P)4] as a tetrahedral shaped starting material for the formation of polymeric coordination compounds
Sebastian Heinl; Konrad Kiefer; Gabor Balazs; Claudia Wickleder; Manfred Scheer; Chem.Commun. 51 (2015) 13474–; doi:10.1039/C5cc04800A

data_7117664
_publ_section_title
;
 The synthesis of the heterocubane cluster [{CpMn}4(mu3-P)4] as a
 tetrahedral shaped starting material for the formation of polymeric
 coordination compounds
;
_journal_name_full               Chem.Commun.
_journal_page_first              13474
_journal_paper_doi               10.1039/C5cc04800A
_journal_volume                  51
_journal_year                    2015
_chemical_compound_source        'see text'
_chemical_formula_moiety         'C34 H30 Mn6 O4 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C36 H34 Cl4 Mn6 O4 P4'
_chemical_formula_weight         1125.95
_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_Int_Tables_number      2
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-03-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-06-03 deposited with the CCDC.
2015-07-10 downloaded from the CCDC.
;
_cell_angle_alpha                77.832(4)
_cell_angle_beta                 80.265(4)
_cell_angle_gamma                85.858(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5319(4)
_cell_length_b                   10.8158(6)
_cell_length_c                   18.0191(8)
_cell_measurement_reflns_used    7767
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      73.3620
_cell_measurement_theta_min      4.1760
_cell_volume                     1976.14(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.12a (release 12-09-2013 CrysAlis171 .NET)
(compiled Sep 12 2013,13:51:24)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.12a (release 12-09-2013 CrysAlis171 .NET)
(compiled Sep 12 2013,13:51:24)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.12a (release 12-09-2013 CrysAlis171 .NET)
(compiled Sep 12 2013,13:51:24)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector_area_resol_mean 5.1773
_diffrn_measured_fraction_theta_full 0.9882
_diffrn_measured_fraction_theta_max 0.9515
_diffrn_measurement_details
;
  1 omega  -98.00   -4.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.9564  125.0000  -60.0000 188

  2 omega   15.00  112.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9564   37.0000 -120.0000 194

  3 omega  -33.00   67.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9564  -37.0000   60.0000 200

  4 omega   79.00  158.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000  -30.0000 158

  5 omega   93.00  120.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000   30.0000 54

  6 omega   41.00  105.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000 -120.0000 128

  7 omega   32.00   71.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000   30.0000 78

  8 omega   25.00  109.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  150.0000 168

  9 omega   81.00  157.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -90.0000 152

 10 omega   29.00   61.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  -30.0000 64

 11 omega   29.00   64.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000  150.0000 70

 12 omega   37.00   63.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000  -90.0000 52

 13 omega   29.00   66.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000    0.0000 74

 14 omega   32.00   77.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  120.0000 90

 15 omega   30.00   68.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000 -180.0000 76

 16 omega   70.00  135.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000  -90.0000 130

 17 omega   90.00  158.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  125.0000 -150.0000 136

 18 omega   43.00  109.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000   60.0000 132

 19 omega   11.00  111.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9564   57.0000  -30.0000 200

 20 omega    7.00  120.00   0.5000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       40.9564   77.0000   60.0000 226
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0016323000
_diffrn_orient_matrix_UB_12      -0.1456149000
_diffrn_orient_matrix_UB_13      0.0221044000
_diffrn_orient_matrix_UB_21      0.1444391000
_diffrn_orient_matrix_UB_22      -0.0053535000
_diffrn_orient_matrix_UB_23      -0.0335035000
_diffrn_orient_matrix_UB_31      0.0345397000
_diffrn_orient_matrix_UB_32      0.0054555000
_diffrn_orient_matrix_UB_33      0.0789536000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14154
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         73.5208
_diffrn_reflns_theta_min         4.18
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.488
_exptl_absorpt_correction_T_max  0.484
_exptl_absorpt_correction_T_min  0.126
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.12a (release 12-09-2013 CrysAlis171 .NET)
(compiled Sep 12 2013,13:51:24)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.1852
_exptl_crystal_size_mid          0.1225
_exptl_crystal_size_min          0.0656
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_Flack   .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         7594
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0619P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0907
_reflns_number_gt                6114
_reflns_number_total             7594
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c5cc04800a2.cif
_cod_data_source_block           1
_cod_database_code               7117664
_chemical_oxdiff_formula         C36H34Mn6P4O4Cl4
_reflns_odcompleteness_completeness 98.82
_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
2. Restrained distances
 Cl3-C36 \\sim Cl4-C36 \\sim Cl3B-C36B \\sim Cl4B-C36B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B: within 1.7A with sigma of 0.01 and
sigma for terminal atoms of 0.01
C11B \\sim C12B \\sim C13B \\sim C14B \\sim C15B: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01
C16B \\sim C17B \\sim C18B \\sim C19B \\sim C20B: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.01
Uanis(C1B) \\sim Ueq, Uanis(C2B) \\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C4B)
\\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C36B) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(Mn1) = Uanis(Mn1B)
4. Others
 Fixed Sof: Mn1(0.75) C1(0.75) H1(0.75) C2(0.75) H2(0.75) C3(0.75) H3(0.75)
 C4(0.75) H4(0.75) C5(0.75) H5(0.75) Mn2(0.75) C6(0.75) H6(0.75) C7(0.75)
 H7(0.75) C8(0.75) H8(0.75) C9(0.75) H9(0.75) C10(0.75) H10(0.75) Mn3(0.75)
 C11(0.75) H11(0.75) C12(0.75) H12(0.75) C13(0.75) H13(0.75) C14(0.75)
 H14(0.75) C15(0.75) H15(0.75) Mn4(0.75) C16(0.75) H16(0.75) C17(0.75)
 H17(0.75) C18(0.75) H18(0.75) C19(0.75) H19(0.75) C20(0.75) H20(0.75) P3(0.75)
 P4(0.75) Mn1B(0.25) C1B(0.25) H1B(0.25) C2B(0.25) H2B(0.25) C3B(0.25)
 H3B(0.25) C4B(0.25) H4B(0.25) C5B(0.25) H5B(0.25) Mn2B(0.25) C6B(0.25)
 H6B(0.25) C7B(0.25) H7B(0.25) C8B(0.25) H8B(0.25) C9B(0.25) H9B(0.25)
 C10B(0.25) H10B(0.25) Mn3B(0.25) C11B(0.25) H11B(0.25) C12B(0.25) H12B(0.25)
 C13B(0.25) H13B(0.25) C14B(0.25) H14B(0.25) C15B(0.25) H15B(0.25) Mn4B(0.25)
 C16B(0.25) H16B(0.25) C17B(0.25) H17B(0.25) C18B(0.25) H18B(0.25) C19B(0.25)
 H19B(0.25) C20B(0.25) H20B(0.25) P3B(0.25) P4B(0.25) C36(0.75) H36A(0.75)
 H36B(0.75) Cl3(0.75) Cl4(0.75) C36B(0.25) H36C(0.25) H36D(0.25) Cl3B(0.25)
 Cl4B(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C36(H36A,H36B), C36B(H36C,H36D)
5.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27),
 C28(H28), C29(H29), C30(H30), C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6),
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C1B(H1B), C2B(H2B),
  C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B), C8B(H8B), C9B(H9B),
 C10B(H10B), C11B(H11B), C12B(H12B), C13B(H13B), C14B(H14B), C15B(H15B),
 C16B(H16B), C17B(H17B), C18B(H18B), C19B(H19B), C20B(H20B)
5.c Fitted pentagon refined as free rotating group:
 C1B(C2B,C3B,C4B,C5B), C6B(C7B,C8B,C9B,C10B), C11B(C12B,C13B,C14B,C15B),
 C16B(C17B,C18B,C19B,C20B)
;
_olex2_submission_special_instructions 'No special instructions were received'