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_7117663
_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         'C27 H25 Mn5 O2 P4, C H2 Cl2'
_chemical_formula_sum            'C28 H27 Cl2 Mn5 O2 P4'
_chemical_formula_weight         864.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.097(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9099(1)
_cell_length_b                   14.8210(1)
_cell_length_c                   17.9552(2)
_cell_measurement_reflns_used    6544
_cell_measurement_temperature    123.05(10)
_cell_measurement_theta_max      66.5629
_cell_measurement_theta_min      2.9791
_cell_volume                     3045.13(5)
_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      123.05(10)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.9864
_diffrn_measured_fraction_theta_max 0.9928
_diffrn_measurement_details
;
  1 omega   65.00  101.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431  145.0000   50.0000 72

  2 omega   14.00  106.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   57.0000 -180.0000 184

  3 omega   66.00  109.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   38.0000   90.0000 86

  4 omega   16.00   68.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -120.0000 104

  5 omega   19.00   67.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000 -180.0000 96

  6 omega   19.00   68.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  120.0000 98

  7 omega   68.00  159.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000  120.0000 182

  8 omega   89.00  119.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  120.0000 60

  9 omega   69.00  162.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000   45.0000    0.0000 186

 10 omega   24.00   72.00   0.5000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -61.0000  120.0000 96

 11 omega  -99.00  -18.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.4431  125.0000   30.0000 162

 12 omega   12.00  109.00   0.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.4431   57.0000  -60.0000 194
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0686730000
_diffrn_orient_matrix_UB_12      0.0336963000
_diffrn_orient_matrix_UB_13      0.0809311000
_diffrn_orient_matrix_UB_21      -0.0755267000
_diffrn_orient_matrix_UB_22      -0.0599315000
_diffrn_orient_matrix_UB_23      0.0371048000
_diffrn_orient_matrix_UB_31      0.0877102000
_diffrn_orient_matrix_UB_32      -0.0780144000
_diffrn_orient_matrix_UB_33      0.0063915000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13200
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        65.7239
_diffrn_reflns_theta_max         66.5629
_diffrn_reflns_theta_min         3.93
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    20.248
_exptl_absorpt_correction_T_max  0.350
_exptl_absorpt_correction_T_min  0.152
_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 brown'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.887
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.1889
_exptl_crystal_size_mid          0.1035
_exptl_crystal_size_min          0.1005
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_Flack   .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     370
_refine_ls_number_reflns         5258
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.867
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0255
_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^)+(0.0312P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0561
_refine_ls_wR_factor_ref         0.0572
_reflns_number_gt                4150
_reflns_number_total             5258
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c5cc04800a2.cif
_cod_data_source_block           1b
_cod_database_code               7117663
_chemical_oxdiff_formula         C28H27Mn5P4Cl2O2
_reflns_odcompleteness_completeness 98.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     65.72
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C2(H2), C9(H9), C21(H21), C20(H20), C1(H1), C3(H3), C10(H10),
 C12(H12), C23(H23), C7(H7), C5(H5), C16(H16), C11(H11), C6(H6), C17(H17),
 C8(H8), C24(H24), C4(H4), C15(H15), C14(H14), C18(H18), C13(H13), C19(H19),
 C25(H25)
;
_olex2_submission_special_instructions 'No special instructions were received'