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_7117661
_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 Br Cu Mn4 P4'
_chemical_formula_sum            'C20 H20 Br Cu Mn4 P4'
_chemical_formula_weight         747.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 101.172(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1032(6)
_cell_length_b                   12.6047(5)
_cell_length_c                   12.7139(4)
_cell_measurement_reflns_used    2877
_cell_measurement_temperature    123.00(14)
_cell_measurement_theta_max      66.0410
_cell_measurement_theta_min      4.7280
_cell_volume                     2217.28(15)
_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(14)
_diffrn_detector_area_resol_mean 10.5431
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega   25.00  107.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3181   38.0000  150.0000 164

  2 omega   35.00  113.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       41.3181   38.0000   60.0000 156

  3 omega   10.00   83.00   0.5000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -94.0000   90.0000 146

  4 omega   16.00   64.00   0.5000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000  -90.0000 96

  5 omega   15.00   95.00   0.5000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -77.0000  120.0000 160

  6 omega   18.00  155.00   0.5000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -15.0000  120.0000 274

  7 omega   27.00   53.00   0.5000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -45.0000    0.0000 52

  8 omega   22.00   67.00   0.5000   70.0000
omega____ theta____ kappa____ phi______ frames
    -       93.5000  -30.0000   90.0000 90
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0926681000
_diffrn_orient_matrix_UB_12      -0.0019412000
_diffrn_orient_matrix_UB_13      -0.0472307000
_diffrn_orient_matrix_UB_21      -0.0575772000
_diffrn_orient_matrix_UB_22      0.0410155000
_diffrn_orient_matrix_UB_23      -0.1076795000
_diffrn_orient_matrix_UB_31      0.0222543000
_diffrn_orient_matrix_UB_32      0.1151177000
_diffrn_orient_matrix_UB_33      0.0378116000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0229
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3838
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.48
_diffrn_reflns_theta_max         66.48
_diffrn_reflns_theta_min         4.75
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.994
_exptl_absorpt_correction_T_max  0.543
_exptl_absorpt_correction_T_min  0.320
_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    2.239
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.078
_exptl_crystal_size_mid          0.0436
_exptl_crystal_size_min          0.0287
_refine_diff_density_max         1.353
_refine_diff_density_min         -1.116
_refine_diff_density_rms         0.226
_refine_ls_abs_structure_details 'Flack H.D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.013(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2437
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0997P)^2^+8.6777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1248
_reflns_number_gt                2370
_reflns_number_total             2437
_reflns_threshold_expression     >2\s(i)
_cod_data_source_file            c5cc04800a2.cif
_cod_data_source_block           1
_cod_database_code               7117661
_chemical_oxdiff_formula         C20H20Mn4P4CuBr
_reflns_odcompleteness_completeness 98.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     65.72
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Br1(0.43) Br2(0.57)
4.a 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'