#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:24:02 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179448 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/45/4334501.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4334501
loop_
_publ_author_name
'Wing-Por Leung'
'Kwok-Wai Kan'
'Yuk-Chi Chan'
'Thomas C. W. Mak'
_publ_section_title
;
 Synthesis of Hetero-Binuclear Complexes from Bisgermavinylidene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4571
_journal_page_last               4577
_journal_paper_doi               10.1021/ic400056f
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C64 H80 Cl8 Ge2 Mn2 N4 P4 Si4'
_chemical_formula_weight         1680.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.300(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.185(2)
_cell_length_b                   13.0651(13)
_cell_length_c                   28.177(3)
_cell_measurement_reflns_used    935
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      3.21
_cell_volume                     8055.5(14)
_computing_cell_refinement       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_collection       'BRUKER SMART CCD DIFFRACTOMETER'
_computing_data_reduction        'BRUKER SMART CCD DIFFRACTOMETER'
_computing_molecular_graphics    'SIEMENS SHELXTL'
_computing_publication_material  'SIEMENS SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'BRUKER SMART CCD DIFFRACTOMETER'
_diffrn_measurement_method       'OMEGA SCAN'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            26699
_diffrn_reflns_theta_full        28.04
_diffrn_reflns_theta_max         28.04
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.488
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.662973
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_density_meas      0
_exptl_crystal_description       Block
_exptl_crystal_F_000             3432
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.876
_refine_diff_density_min         -0.746
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         9703
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0417
_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/[σ²(Fo²)+(0.0628P)²+10.7587P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1108
_refine_ls_wR_factor_ref         0.1265
_reflns_number_gt                7092
_reflns_number_total             9703
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400056f_si_005.cif
_cod_data_source_block           kkw64
_cod_database_code               4334501
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ge1 Ge -0.438576(14) 0.81067(2) 0.544827(12) 0.04054(10) Uani 1 1 d .
Mn1 Mn -0.30569(2) 0.80206(3) 0.523113(17) 0.03959(12) Uani 1 1 d .
P1 P -0.36729(3) 0.71904(5) 0.62759(3) 0.03265(15) Uani 1 1 d .
P2 P -0.30796(3) 0.92792(5) 0.60657(2) 0.03247(15) Uani 1 1 d .
Si1 Si -0.49750(4) 0.61812(7) 0.58691(3) 0.0475(2) Uani 1 1 d .
Si2 Si -0.26729(5) 1.06210(8) 0.53657(4) 0.0593(3) Uani 1 1 d .
Cl1 Cl -0.40485(4) 0.72353(8) 0.47744(3) 0.0570(2) Uani 1 1 d .
Cl2 Cl -0.22276(4) 0.68161(7) 0.55537(3) 0.0512(2) Uani 1 1 d .
Cl3 Cl -0.54709(15) 0.9906(2) 0.63828(16) 0.2521(17) Uani 1 1 d .
Cl4 Cl -0.5478(2) 1.1541(4) 0.69500(18) 0.307(2) Uani 1 1 d .
N1 N -0.43339(11) 0.68800(18) 0.58761(9) 0.0378(5) Uani 1 1 d .
N2 N -0.29249(11) 0.95037(18) 0.55622(8) 0.0377(5) Uani 1 1 d .
C1 C -0.54457(17) 0.6081(4) 0.51905(14) 0.0735(11) Uani 1 1 d .
H1A H -0.5219 0.5723 0.5013 0.110 Uiso 1 1 calc R
H1B H -0.5545 0.6755 0.5052 0.110 Uiso 1 1 calc R
H1C H -0.5816 0.5714 0.5158 0.110 Uiso 1 1 calc R
C2 C -0.4768(2) 0.4900(3) 0.61538(18) 0.0872(14) Uani 1 1 d .
H2A H -0.4528 0.4973 0.6502 0.131 Uiso 1 1 calc R
H2B H -0.4535 0.4540 0.5982 0.131 Uiso 1 1 calc R
H2C H -0.5133 0.4522 0.6125 0.131 Uiso 1 1 calc R
C3 C -0.5412(2) 0.6874(4) 0.62149(19) 0.0892(15) Uani 1 1 d .
H3A H -0.5171 0.6918 0.6564 0.134 Uiso 1 1 calc R
H3B H -0.5784 0.6511 0.6180 0.134 Uiso 1 1 calc R
H3C H -0.5507 0.7551 0.6079 0.134 Uiso 1 1 calc R
C4 C -0.35251(12) 0.8194(2) 0.59420(10) 0.0335(5) Uani 1 1 d .
C5 C -0.3268(3) 1.1074(5) 0.4790(2) 0.141(3) Uani 1 1 d .
H5A H -0.3365 1.0540 0.4542 0.212 Uiso 1 1 calc R
H5B H -0.3122 1.1662 0.4661 0.212 Uiso 1 1 calc R
H5C H -0.3629 1.1254 0.4868 0.212 Uiso 1 1 calc R
C6 C -0.1959(2) 1.0369(4) 0.5221(2) 0.0947(16) Uani 1 1 d .
H6A H -0.2034 0.9846 0.4969 0.142 Uiso 1 1 calc R
H6B H -0.1645 1.0144 0.5521 0.142 Uiso 1 1 calc R
H6C H -0.1830 1.0985 0.5100 0.142 Uiso 1 1 calc R
C7 C -0.2477(3) 1.1646(4) 0.5856(2) 0.121(2) Uani 1 1 d .
H7A H -0.2830 1.1807 0.5947 0.181 Uiso 1 1 calc R
H7B H -0.2344 1.2247 0.5726 0.181 Uiso 1 1 calc R
H7C H -0.2155 1.1410 0.6148 0.181 Uiso 1 1 calc R
C11 C -0.37614(13) 0.7489(2) 0.68767(10) 0.0396(6) Uani 1 1 d .
C12 C -0.36489(18) 0.6785(3) 0.72607(12) 0.0567(9) Uani 1 1 d .
H12A H -0.3473 0.6156 0.7234 0.068 Uiso 1 1 calc R
C13 C -0.3799(2) 0.7015(4) 0.76901(15) 0.0766(12) Uani 1 1 d .
H13A H -0.3722 0.6537 0.7948 0.092 Uiso 1 1 calc R
C14 C -0.4056(2) 0.7934(3) 0.77339(15) 0.0716(12) Uani 1 1 d .
H14A H -0.4152 0.8081 0.8022 0.086 Uiso 1 1 calc R
C15 C -0.41729(17) 0.8641(3) 0.73543(14) 0.0613(9) Uani 1 1 d .
H15A H -0.4349 0.9267 0.7384 0.074 Uiso 1 1 calc R
C16 C -0.40280(15) 0.8418(3) 0.69252(12) 0.0486(7) Uani 1 1 d .
H16A H -0.4110 0.8896 0.6667 0.058 Uiso 1 1 calc R
C21 C -0.31412(14) 0.6135(2) 0.63927(11) 0.0406(6) Uani 1 1 d .
C22 C -0.25768(16) 0.6195(3) 0.67725(13) 0.0558(8) Uani 1 1 d .
H22A H -0.2474 0.6769 0.6978 0.067 Uiso 1 1 calc R
C23 C -0.2165(2) 0.5380(4) 0.68416(17) 0.0759(12) Uani 1 1 d .
H23A H -0.1787 0.5416 0.7094 0.091 Uiso 1 1 calc R
C24 C -0.2314(2) 0.4538(4) 0.65427(18) 0.0843(14) Uani 1 1 d .
H24A H -0.2041 0.3996 0.6594 0.101 Uiso 1 1 calc R
C25 C -0.2866(2) 0.4488(3) 0.61668(17) 0.0774(12) Uani 1 1 d .
H25A H -0.2965 0.3910 0.5963 0.093 Uiso 1 1 calc R
C26 C -0.32779(17) 0.5287(3) 0.60869(13) 0.0545(8) Uani 1 1 d .
H26A H -0.3649 0.5252 0.5826 0.065 Uiso 1 1 calc R
C31 C -0.34744(14) 1.0370(2) 0.62191(11) 0.0412(6) Uani 1 1 d .
C32 C -0.39986(16) 1.0707(3) 0.58512(14) 0.0585(9) Uani 1 1 d .
H32A H -0.4135 1.0369 0.5544 0.070 Uiso 1 1 calc R
C33 C -0.4324(2) 1.1538(3) 0.59324(18) 0.0801(13) Uani 1 1 d .
H33A H -0.4666 1.1771 0.5676 0.096 Uiso 1 1 calc R
C34 C -0.4141(3) 1.2018(4) 0.6392(2) 0.1000(17) Uani 1 1 d .
H34A H -0.4362 1.2571 0.6450 0.120 Uiso 1 1 calc R
C35 C -0.3641(3) 1.1682(4) 0.67566(19) 0.1002(18) Uani 1 1 d .
H35A H -0.3523 1.1997 0.7070 0.120 Uiso 1 1 calc R
C36 C -0.3298(2) 1.0877(3) 0.66740(14) 0.0698(11) Uani 1 1 d .
H36A H -0.2945 1.0676 0.6928 0.084 Uiso 1 1 calc R
C41 C -0.23890(13) 0.9101(2) 0.66034(11) 0.0411(6) Uani 1 1 d .
C42 C -0.23877(16) 0.9004(2) 0.70979(11) 0.0507(8) Uani 1 1 d .
H42A H -0.2756 0.8991 0.7162 0.061 Uiso 1 1 calc R
C43 C -0.1844(2) 0.8926(3) 0.74914(14) 0.0666(10) Uani 1 1 d .
H43A H -0.1848 0.8879 0.7819 0.080 Uiso 1 1 calc R
C44 C -0.1303(2) 0.8918(4) 0.74039(16) 0.0809(13) Uani 1 1 d .
H44A H -0.0939 0.8868 0.7671 0.097 Uiso 1 1 calc R
C45 C -0.12925(18) 0.8983(4) 0.69180(18) 0.0836(13) Uani 1 1 d .
H45A H -0.0922 0.8966 0.6857 0.100 Uiso 1 1 calc R
C46 C -0.18344(16) 0.9075(3) 0.65208(14) 0.0623(9) Uani 1 1 d .
H46A H -0.1825 0.9119 0.6194 0.075 Uiso 1 1 calc R
C51 C -0.5770(3) 1.1039(9) 0.6352(3) 0.200(5) Uani 1 1 d .
H51A H -0.6212 1.0995 0.6247 0.240 Uiso 1 1 calc R
H51B H -0.5658 1.1463 0.6113 0.240 Uiso 1 1 calc R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Ge1 C4 77.28(10) . .
N1 Ge1 Cl1 96.88(7) . .
C4 Ge1 Cl1 93.53(8) . .
N1 Ge1 P1 37.60(7) . .
C4 Ge1 P1 40.15(7) . .
Cl1 Ge1 P1 101.40(3) . .
N2 Mn1 Cl2 116.52(7) . .
N2 Mn1 Cl1 125.72(7) . .
Cl2 Mn1 Cl1 114.54(4) . .
N2 Mn1 Cl2 105.45(6) . 7_466
Cl2 Mn1 Cl2 88.78(3) . 7_466
Cl1 Mn1 Cl2 92.68(3) . 7_466
N2 Mn1 C4 67.48(8) . .
Cl2 Mn1 C4 104.55(6) . .
Cl1 Mn1 C4 83.26(6) . .
Cl2 Mn1 C4 166.59(6) 7_466 .
N2 Mn1 P2 33.10(6) . .
Cl2 Mn1 P2 106.93(3) . .
Cl1 Mn1 P2 113.52(3) . .
Cl2 Mn1 P2 138.48(3) 7_466 .
C4 Mn1 P2 36.16(6) . .
N1 P1 C4 97.14(12) . .
N1 P1 C21 111.48(13) . .
C4 P1 C21 115.86(13) . .
N1 P1 C11 109.21(13) . .
C4 P1 C11 116.93(13) . .
C21 P1 C11 105.97(13) . .
N1 P1 Ge1 48.18(8) . .
C4 P1 Ge1 49.63(9) . .
C21 P1 Ge1 133.90(10) . .
C11 P1 Ge1 119.53(10) . .
N2 P2 C4 105.47(12) . .
N2 P2 C41 111.61(13) . .
C4 P2 C41 111.56(13) . .
N2 P2 C31 110.13(13) . .
C4 P2 C31 112.21(14) . .
C41 P2 C31 105.98(14) . .
N2 P2 Mn1 46.55(9) . .
C4 P2 Mn1 62.39(9) . .
C41 P2 Mn1 110.98(10) . .
C31 P2 Mn1 141.78(10) . .
N1 Si1 C2 111.83(17) . .
N1 Si1 C3 110.54(17) . .
C2 Si1 C3 108.8(2) . .
N1 Si1 C1 104.85(15) . .
C2 Si1 C1 111.2(2) . .
C3 Si1 C1 109.6(2) . .
N2 Si2 C5 108.5(2) . .
N2 Si2 C6 109.85(18) . .
C5 Si2 C6 109.0(3) . .
N2 Si2 C7 113.16(18) . .
C5 Si2 C7 110.4(3) . .
C6 Si2 C7 105.8(3) . .
Mn1 Cl1 Ge1 83.54(3) . .
Mn1 Cl2 Mn1 91.22(3) . 7_466
P1 N1 Si1 138.20(15) . .
P1 N1 Ge1 94.21(11) . .
Si1 N1 Ge1 122.48(13) . .
P2 N2 Si2 129.52(15) . .
P2 N2 Mn1 100.35(11) . .
Si2 N2 Mn1 130.00(13) . .
P1 C4 P2 137.32(16) . .
P1 C4 Ge1 90.22(12) . .
P2 C4 Ge1 125.09(14) . .
P1 C4 Mn1 124.77(13) . .
P2 C4 Mn1 81.45(10) . .
Ge1 C4 Mn1 91.92(10) . .
C12 C11 C16 118.8(3) . .
C12 C11 P1 122.6(2) . .
C16 C11 P1 118.1(2) . .
C11 C12 C13 120.0(3) . .
C14 C13 C12 120.6(4) . .
C13 C14 C15 120.2(3) . .
C14 C15 C16 119.7(4) . .
C15 C16 C11 120.8(3) . .
C26 C21 C22 119.4(3) . .
C26 C21 P1 119.9(2) . .
C22 C21 P1 120.6(2) . .
C21 C22 C23 119.3(4) . .
C24 C23 C22 120.5(4) . .
C23 C24 C25 120.1(4) . .
C24 C25 C26 120.6(4) . .
C21 C26 C25 120.2(4) . .
C36 C31 C32 117.4(3) . .
C36 C31 P2 125.3(3) . .
C32 C31 P2 117.2(2) . .
C31 C32 C33 121.2(4) . .
C34 C33 C32 119.9(4) . .
C35 C34 C33 119.4(4) . .
C34 C35 C36 121.2(4) . .
C31 C36 C35 120.7(4) . .
C46 C41 C42 118.1(3) . .
C46 C41 P2 118.4(2) . .
C42 C41 P2 123.6(2) . .
C43 C42 C41 120.5(4) . .
C44 C43 C42 120.6(4) . .
C43 C44 C45 120.0(4) . .
C44 C45 C46 119.9(4) . .
C41 C46 C45 120.8(4) . .
Cl3 C51 Cl4 105.7(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 N1 1.985(2) .
Ge1 C4 2.024(3) .
Ge1 Cl1 2.5485(9) .
Ge1 P1 2.6562(8) .
Mn1 N2 2.128(2) .
Mn1 Cl2 2.4176(9) .
Mn1 Cl1 2.4573(9) .
Mn1 Cl2 2.5170(9) 7_466
Mn1 C4 2.584(3) .
Mn1 P2 2.8841(8) .
P1 N1 1.625(2) .
P1 C4 1.713(3) .
P1 C21 1.806(3) .
P1 C11 1.814(3) .
P2 N2 1.601(2) .
P2 C4 1.721(3) .
P2 C41 1.819(3) .
P2 C31 1.822(3) .
Si1 N1 1.739(2) .
Si1 C2 1.850(4) .
Si1 C3 1.857(4) .
Si1 C1 1.867(4) .
Si2 N2 1.730(2) .
Si2 C5 1.845(5) .
Si2 C6 1.860(5) .
Si2 C7 1.869(5) .
Cl2 Mn1 2.5170(9) 7_466
Cl3 C51 1.624(11) .
Cl4 C51 1.725(10) .
C11 C12 1.378(4) .
C11 C16 1.389(4) .
C12 C13 1.397(5) .
C13 C14 1.364(6) .
C14 C15 1.371(6) .
C15 C16 1.389(4) .
C21 C26 1.374(4) .
C21 C22 1.392(4) .
C22 C23 1.399(5) .
C23 C24 1.359(7) .
C24 C25 1.365(7) .
C25 C26 1.384(5) .
C31 C36 1.379(4) .
C31 C32 1.383(4) .
C32 C33 1.384(5) .
C33 C34 1.374(7) .
C34 C35 1.343(7) .
C35 C36 1.384(6) .
C41 C46 1.381(5) .
C41 C42 1.398(4) .
C42 C43 1.381(5) .
C43 C44 1.356(6) .
C44 C45 1.380(6) .
C45 C46 1.384(5) .
