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_7117666
_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         'C48 H40 Mn8 O8 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C50 H44 Cl4 Mn8 O8 P4'
_chemical_formula_weight         1478.05
_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                 132.060(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.4777(8)
_cell_length_b                   11.0635(3)
_cell_length_c                   21.2608(6)
_cell_measurement_reflns_used    7480
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.4760
_cell_measurement_theta_min      3.9920
_cell_volume                     5147.9(4)
_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      123.01(10)
_diffrn_detector_area_resol_mean 10.3546
_diffrn_measured_fraction_theta_full 0.9868
_diffrn_measured_fraction_theta_max 0.9484
_diffrn_measurement_details
;
  1 omega  -94.00   -6.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  125.0000   60.0000 176

  2 omega   25.00   96.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   37.0000  -30.0000 142

  3 omega   77.00  105.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   85.0000 -161.0000 56

  4 omega   33.00  121.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000   30.0000 176

  5 omega   89.00  158.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000 -120.0000 138

  6 omega   34.00  109.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000   90.0000 150

  7 omega   75.00  151.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  -60.0000 152

  8 omega   37.00   75.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000  120.0000 76

  9 omega   76.00  101.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000 -150.0000 50

 10 omega  125.00  152.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000 -150.0000 54

 11 omega   29.00   55.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -30.0000   60.0000 52

 12 omega -123.00    5.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -19.0000   60.0000 256

 13 omega -120.00   -8.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000   30.0000 224

 14 omega   12.00  115.00   0.5000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       41.2064   57.0000 -150.0000 206

 15 omega   32.00   76.00   0.5000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000 -150.0000 88
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0473297000
_diffrn_orient_matrix_UB_12      0.0790102000
_diffrn_orient_matrix_UB_13      0.0095326000
_diffrn_orient_matrix_UB_21      -0.0404270000
_diffrn_orient_matrix_UB_22      0.1120847000
_diffrn_orient_matrix_UB_23      -0.0267602000
_diffrn_orient_matrix_UB_31      0.0328714000
_diffrn_orient_matrix_UB_32      0.0241690000
_diffrn_orient_matrix_UB_33      0.0933709000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13730
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         73.5826
_diffrn_reflns_theta_min         4.04
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    18.978
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_correction_T_min  0.443
_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            black
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.907
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.067
_exptl_crystal_size_mid          0.0411
_exptl_crystal_size_min          0.0365
_refine_diff_density_max         1.174
_refine_diff_density_min         -1.068
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_Flack   .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.988
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0402P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0652
_refine_ls_wR_factor_ref         0.0667
_reflns_number_gt                4070
_reflns_number_total             4948
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c5cc04800a2.cif
_cod_data_source_block           1d
_cod_database_code               7117666
_chemical_oxdiff_formula         C50H44Cl4Mn8P4O8
_reflns_odcompleteness_completeness 98.68
_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.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
2.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)
;
_olex2_submission_special_instructions 'No special instructions were received'