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_7117665
_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         '2(C41 H35 Mn7 O6 P4), 3(C H2 Cl2)'
_chemical_formula_sum            'C85 H76 Cl6 Mn14 O12 P8'
_chemical_formula_weight         2519.08
_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                79.072(1)
_cell_angle_beta                 82.668(1)
_cell_angle_gamma                83.529(1)
_cell_formula_units_Z            1
_cell_length_a                   10.3548(2)
_cell_length_b                   10.5563(1)
_cell_length_c                   20.4728(3)
_cell_measurement_reflns_used    15567
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      73.4810
_cell_measurement_theta_min      4.2530
_cell_volume                     2170.28(6)
_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 0.9923
_diffrn_measured_fraction_theta_max 0.9606
_diffrn_measurement_details
;
  1 omega -115.00  -22.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000 -150.0000 186

  2 omega  -62.00   35.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064   37.0000    0.0000 194

  3 omega   12.00   97.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2064 -125.0000  120.0000 170

  4 omega -125.00  -73.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000 -125.0000  -30.0000 104

  5 omega   70.00  101.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  -30.0000 62

  6 omega   34.00   76.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -45.0000   60.0000 84

  7 omega   32.00   58.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000  -90.0000 52

  8 omega   88.00  157.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000   30.0000 138

  9 omega   23.00   48.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000  -30.0000 50

 10 omega   33.00  135.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -61.0000  120.0000 204

 11 omega   28.00   93.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000  -90.0000 130

 12 omega  104.00  141.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -77.0000  -90.0000 74

 13 omega   84.00  109.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000    0.0000 50

 14 omega   21.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800    0.0000 -150.0000 274

 15 omega   23.00   63.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000    0.0000 80

 16 omega   26.00  109.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800  -94.0000   90.0000 166

 17 omega   71.00  121.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800 -125.0000  -90.0000 100

 18 omega -120.00   -8.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000  -60.0000 224

 19 omega -115.00  -12.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -57.0000    0.0000 206

 20 omega -120.00   -8.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000  120.0000 224

 21 omega -162.00  -49.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000   60.0000 226

 22 omega -162.00  -49.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -83.0000  -77.0000  150.0000 226

 23 omega   73.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   77.0000  -90.0000 170

 24 omega   79.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   45.0000 -120.0000 158

 25 omega   77.00  158.00   0.5000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      106.9800   61.0000  -30.0000 162

 26 omega -117.00  -58.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -37.0000  120.0000 118

 27 omega -120.00   -8.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000   30.0000 224

 28 omega  -98.00   -2.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  125.0000  120.0000 192

 29 omega -120.00   -8.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -      -41.2064  -77.0000 -150.0000 224

 30 omega    2.00   24.00   0.5000    1.5000
omega____ theta____ kappa____ phi______ frames
    -       41.2064 -125.0000 -120.0000 44
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0955986000
_diffrn_orient_matrix_UB_12      -0.0558513000
_diffrn_orient_matrix_UB_13      -0.0537160000
_diffrn_orient_matrix_UB_21      -0.0562279000
_diffrn_orient_matrix_UB_22      0.1049466000
_diffrn_orient_matrix_UB_23      -0.0547569000
_diffrn_orient_matrix_UB_31      0.1019222000
_diffrn_orient_matrix_UB_32      0.0902371000
_diffrn_orient_matrix_UB_33      0.0077666000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0290
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26928
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         73.5017
_diffrn_reflns_theta_min         4.28
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    19.547
_exptl_absorpt_correction_T_max  0.532
_exptl_absorpt_correction_T_min  0.058
_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    1.927
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plank
_exptl_crystal_F_000             1254
_exptl_crystal_size_max          0.3779
_exptl_crystal_size_mid          0.0484
_exptl_crystal_size_min          0.0379
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.025
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_Flack   .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8389
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0732P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1019
_reflns_number_gt                7451
_reflns_number_total             8389
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c5cc04800a2.cif
_cod_data_source_block           1c
_cod_database_code               7117665
_chemical_oxdiff_formula         C42.5H38O6P4Mn7Cl3
_reflns_odcompleteness_completeness 99.23
_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. Others
 Fixed Sof: C43(0.5) H43A(0.5) H43B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 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)
;
_olex2_submission_special_instructions 'No special instructions were received'