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_7117660
_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         'C20 H20 Mn4 P4, C H2 Cl2'
_chemical_formula_sum            'C21 H22 Cl2 Mn4 P4'
_chemical_formula_weight         688.93
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                90
_cell_angle_beta                 116.922(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   40.9164(6)
_cell_length_b                   9.3302(1)
_cell_length_c                   27.2353(4)
_cell_measurement_reflns_used    18003
_cell_measurement_temperature    123.1(6)
_cell_measurement_theta_max      66.4324
_cell_measurement_theta_min      3.6272
_cell_volume                     9270.5(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_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      123.1(6)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -47.00  -21.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4431  125.0000  150.0000 52

  2 omega   13.00   92.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431 -125.0000  120.0000 158

  3 omega   21.00  117.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   38.0000   60.0000 192

  4 omega   12.00   81.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000    0.0000 138

  5 omega   96.00  167.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  -90.0000 142

  6 omega   24.00   84.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000  120.0000 120

  7 omega   23.00   66.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -180.0000 86

  8 omega   10.00   82.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000   60.0000 144

  9 omega   28.00   93.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000 -125.0000 -150.0000 130

 10 omega   46.00   87.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   15.0000  -90.0000 82

 11 omega   28.00   78.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000 -150.0000 100

 12 omega   13.00   80.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -95.0000   90.0000 134

 13 omega   27.00   72.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000 -180.0000 90

 14 omega  -71.00   33.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4431   57.0000    0.0000 208

 15 omega   15.00  117.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   38.0000 -180.0000 204

 16 omega   12.00  115.00   0.5000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   57.0000  -60.0000 206

 17 omega   66.00   95.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000   90.0000 58
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0169605000
_diffrn_orient_matrix_UB_12      0.1426827000
_diffrn_orient_matrix_UB_13      0.0055772000
_diffrn_orient_matrix_UB_21      0.0187748000
_diffrn_orient_matrix_UB_22      -0.0172764000
_diffrn_orient_matrix_UB_23      0.0630924000
_diffrn_orient_matrix_UB_31      0.0337975000
_diffrn_orient_matrix_UB_32      0.0813043000
_diffrn_orient_matrix_UB_33      0.0036143000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            25380
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.54
_diffrn_reflns_theta_max         66.54
_diffrn_reflns_theta_min         3.64
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    22.144
_exptl_absorpt_correction_T_max  0.574
_exptl_absorpt_correction_T_min  0.032
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
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 red'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.974
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             5472
_exptl_crystal_size_max          0.5337
_exptl_crystal_size_mid          0.1091
_exptl_crystal_size_min          0.0262
_refine_diff_density_max         0.957
_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.136
_refine_ls_abs_structure_Flack   .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         8019
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.0425
_refine_ls_R_factor_gt           0.0390
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0783P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1010
_refine_ls_wR_factor_ref         0.1021
_reflns_number_gt                6872
_reflns_number_total             8019
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5cc04800a2.cif
_cod_data_source_block           1
_cod_database_code               7117660
_chemical_oxdiff_formula         C42H44Mn8P8Cl4
_reflns_odcompleteness_completeness 96.85
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C13) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C19)
\\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004
3.a Secondary CH2 refined with riding coordinates:
 C41(H41A,H41B), C42(H42A,H42B)
3.b Aromatic/amide H refined with riding coordinates:
 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), C21(H21), C22(H22), C23(H23), C24(H24),
 C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32),
  C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
;
_olex2_submission_special_instructions 'No special instructions were received'