Multicomponent Self-Assembly of Thiolato- and Selenato-Bridged Ester-Functionalized Rhenium(I)-Based Trigonal Metallaprisms: Synthesis and Structural Characterization
Nagarajaprakash, R.; Ashok Kumar, Chowan; Mobin, Shaikh M.; Manimaran, Bala.; Organometallics 34 (2015) 724–; doi:10.1021/om501005n

data_4085392
_publ_section_title
;
 Multicomponent Self-Assembly of Thiolato- and Selenato-Bridged
 Ester-Functionalized Rhenium(I)-Based Trigonal Metallaprisms: Synthesis
 and Structural Characterization
;
_journal_issue                   4
_journal_name_full               Organometallics
_journal_page_first              724
_journal_paper_doi               10.1021/om501005n
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety
'2(C102 H60 N6 O30 Re6 Se6), 16(C3 H7 N O), C2 H4 N O'
_chemical_formula_sum            'C254 H236 N29 O77 Re12 Se12'
_chemical_formula_weight         8108.64
_chemical_name_systematic
;
 ?
;
_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_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             2013-03-19
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                114.0778(15)
_cell_angle_beta                 103.6009(13)
_cell_angle_gamma                90.4509(12)
_cell_formula_units_Z            1
_cell_length_a                   14.3173(2)
_cell_length_b                   23.7212(4)
_cell_length_c                   24.7775(4)
_cell_measurement_temperature    293(2)
_cell_volume                     7416.1(2)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            82104
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.64
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.427
_exptl_absorpt_correction_T_max  0.189
_exptl_absorpt_correction_T_min  0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.816
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3887
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_refine_diff_density_max         4.705
_refine_diff_density_min         -3.622
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1691
_refine_ls_number_reflns         26056
_refine_ls_number_restraints     1623
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0503
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+93.6386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1251
_reflns_number_gt                21873
_reflns_number_total             26056
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501005n_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 4085391--4085392.cif.'
_cod_database_code               4085392
_olex2_refinement_description
;
1. Others
 Fixed Sof: C3V(0.5) H3VA(0.5) H3VB(0.5) H3VC(0.5) O39(0.5) N3V(0.5) C1A(0.5)
 H1A(0.5)
 Fixed Uiso: H70(0.034) H88(0.028) H82(0.028) H80(0.025) H86(0.029) H59(0.03)
 H102(0.036) H71(0.037) H58(0.028) H79(0.025) H100(0.028) H66(0.032)
 H101(0.032) H83(0.027) H99(0.028) H62(0.03) H90(0.029) H72(0.04) H64(0.03)
 H55(0.033) H29(0.041) H32(0.037) H56(0.033) H69(0.035) H36(0.033) H30(0.039)
 H24(0.038) H35(0.044) H96(0.044) H27(0.047) H93(0.05) H34(0.047) H95(0.046)
 H26(0.041) H33(0.044) H28(0.044) H78(0.044) H38(0.044) H77(0.046) H42(0.051)
 H94(0.053) H22(0.061) H40(0.061) H39(0.059) H41(0.058) H23(0.052) H20(0.054)
 H21(0.071) H48(0.066) H75(0.078) H50(0.084) H51(0.093) H52(0.083) H53(0.093)
 H54(0.084) H44(0.072) H76(0.089) H47(0.079) H46(0.088) H45(0.083) H11A(0.11)
 H11B(0.11) H11C(0.11) H114(0.069) H111(0.059) H11G(0.093) H11H(0.093)
 H11I(0.093) H11J(0.103) H11K(0.103) H11L(0.103) H11M(0.093) H11N(0.093)
 H11O(0.093) H12A(0.107) H120(0.107) H117(0.14) H11D(0.133) H11E(0.133)
 H11F(0.133) H123(0.123) H3VA(0.094) H3VB(0.094) H3VC(0.094) H10M(0.167)
 H10N(0.167) H10O(0.167) H12B(0.195) H12C(0.195) H12D(0.195) H126(0.149)
 H11P(0.174) H11Q(0.174) H11R(0.174) H108(0.156) H10A(0.181) H10B(0.181)
 H10C(0.181) H12H(0.229) H12I(0.229) H12J(0.229) H12K(0.256) H12L(0.256)
 H12M(0.256) H11S(0.174) H11T(0.174) H11U(0.174) H10D(0.247) H10E(0.247)
 H10F(0.247) H1A(0.075) H12E(0.425) H12F(0.425) H12G(0.425) H105(0.079)
 H142(0.079) H10G(0.137) H10H(0.137) H10I(0.137) H10J(0.134) H10K(0.134)
 H10L(0.134) H14A(0.137) H14B(0.137) H14C(0.137) H14D(0.134) H14E(0.134)
 H14F(0.134)
 Fixed X: H70(0.2079) H88(0.1724) H82(0.3455) H80(0.0722) H86(0.2779)
 H59(0.224) H102(-0.0183) H71(0.2276) H58(0.2049) H79(0.1191) H100(-0.0224)
 H66(0.3393) H101(-0.0818) H83(0.3843) H99(0.0504) H62(0.4775) H90(0.1532)
 H72(0.2911) H64(0.4111) H55(0.4991) H29(0.6628) H32(-0.1061) H56(0.488)
 H69(0.269) H36(0.0048) H30(0.5489) H24(0.1317) H35(-0.0662) H96(0.386)
 H27(0.6599) H93(0.3157) H34(-0.1576) H95(0.4442) H26(0.5432) H33(-0.1798)
 H28(0.7168) H78(0.5869) H38(-0.144) H77(0.6669) H42(0.128) H94(0.3772)
 H22(0.0086) H40(-0.0486) H39(-0.1721) H41(0.1022) H23(0.0446) H20(0.1476)
 H21(0.0585) H48(0.6017) H75(0.5506) H50(0.6025) H51(0.6299) H52(0.6575)
 H53(0.6462) H54(0.6175) H44(0.8457) H76(0.6315) H47(0.6876) H46(0.8523)
 H45(0.9302) H11A(0.4713) H11B(0.4447) H11C(0.5143) H114(0.9974) H111(0.6497)
 H11G(0.7276) H11H(0.748) H11I(0.7839) H11J(0.8522) H11K(0.811) H11L(0.9231)
 H11M(0.8478) H11N(0.9153) H11O(0.8993) H12A(0.3192) H120(0.445) H117(0.4752)
 H11D(0.2905) H11E(0.2378) H11F(0.2521) H123(0.1947) H3VA(0.4373) H3VB(0.4962)
 H3VC(0.4241) H10M(0.8381) H10N(0.8538) H10O(0.7507) H12B(0.179) H12C(0.1303)
 H12D(0.0663) H126(0.8732) H11P(0.3669) H11Q(0.3955) H11R(0.4238) H108(0.022)
 H10A(-0.124) H10B(-0.2204) H10C(-0.165) H12H(0.7963) H12I(0.8405) H12J(0.9077)
 H12K(0.9325) H12L(0.8293) H12M(0.9169) H11S(0.6145) H11T(0.5735) H11U(0.6444)
 H10D(-0.1826) H10E(-0.1961) H10F(-0.1033) H1A(0.6451) H12E(0.0098)
 H12F(0.0938) H12G(0.0864) H105(0.5409) H142(0.56) H10G(0.5534) H10H(0.5663)
 H10I(0.4629) H10J(0.4208) H10K(0.5285) H10L(0.4937) H14A(0.5612) H14B(0.5348)
 H14C(0.4534) H14D(0.4781) H14E(0.4664) H14F(0.5676)
 Fixed Y: H70(-0.273) H88(0.0336) H82(0.2403) H80(0.2113) H86(0.1974)
 H59(0.1408) H102(-0.134) H71(-0.2933) H58(0.0925) H79(0.2711) H100(-0.2211)
 H66(-0.02) H101(-0.2358) H83(0.3004) H99(-0.1211) H62(0.1474) H90(0.0595) H72(-
 0.1919) H64(0.0155) H55(0.1885) H29(0.4147) H32(-0.3361) H56(0.1421) H69(-
 0.1696) H36(-0.4825) H30(0.3367) H24(0.3797) H35(-0.5443) H96(0.0751)
 H27(0.5056) H93(0.2316) H34(-0.503) H95(0.1333) H26(0.4306) H33(-0.399)
 H28(0.4989) H78(0.1216) H38(-0.4439) H77(0.164) H42(-0.4083) H94(0.285)
 H22(0.331) H40(-0.5405) H39(-0.5222) H41(-0.4862) H23(0.404) H20(0.2091)
 H21(0.2339) H48(0.1423) H75(0.2942) H50(0.4239) H51(0.5327) H52(0.5967)
 H53(0.5578) H54(0.4507) H44(0.2266) H76(0.3316) H47(0.1097) H46(0.1352)
 H45(0.1997) H11A(0.4281) H11B(0.4559) H11C(0.4958) H114(0.2946) H111(0.2819)
 H11G(0.2632) H11H(0.3087) H11I(0.2427) H11J(0.3919) H11K(0.3476) H11L(0.3637)
 H11M(0.2079) H11N(0.269) H11O(0.2485) H12A(0.5487) H120(0.5572) H117(0.9843)
 H11D(0.4072) H11E(0.4548) H11F(0.4636) H123(0.9418) H3VA(1.0424) H3VB(1.0505)
 H3VC(0.9903) H10M(0.3591) H10N(0.3688) H10O(0.3706) H12B(0.7858) H12C(0.7725)
 H12D(0.7823) H126(0.66) H11P(0.9526) H11Q(0.9609) H11R(0.9035) H108(0.0347)
 H10A(0.1322) H10B(0.1009) H10C(0.0642) H12H(0.7633) H12I(0.7343) H12J(0.7761)
 H12K(0.6418) H12L(0.6098) H12M(0.6052) H11S(0.9679) H11T(1.0314) H11U(1.0243)
 H10D(0.0203) H10E(0.0912) H10F(0.0689) H1A(0.9395) H12E(0.8746) H12F(0.873)
 H12G(0.933) H105(0.2952) H142(0.3739) H10G(0.3629) H10H(0.4296) H10I(0.3984)
 H10J(0.4075) H10K(0.4375) H10L(0.3758) H14A(0.4433) H14B(0.4204) H14C(0.421)
 H14D(0.2661) H14E(0.3156) H14F(0.2927)
 Fixed Z: H70(0.3336) H88(0.6012) H82(0.4768) H80(0.3744) H86(0.6127)
 H59(0.2262) H102(0.3195) H71(0.4844) H58(0.2874) H79(0.33) H100(0.4526)
 H66(0.4093) H101(0.2847) H83(0.4307) H99(0.4907) H62(0.5352) H90(0.4475)
 H72(0.542) H64(0.5877) H55(0.3108) H29(0.2547) H32(0.4937) H56(0.3753)
 H69(0.3888) H36(0.3874) H30(0.2419) H24(0.2261) H35(0.4226) H96(0.7951)
 H27(0.4297) H93(0.7806) H34(0.4907) H95(0.8994) H26(0.417) H33(0.5259)
 H28(0.3477) H78(0.7306) H38(0.1849) H77(0.8348) H42(0.1844) H94(0.8849)
 H22(0.0485) H40(0.0374) H39(0.0852) H41(0.0877) H23(0.1499) H20(0.1029)
 H21(0.0257) H48(1.0362) H75(0.7473) H50(1.0961) H51(1.1545) H52(1.1117)
 H53(1.0088) H54(0.9488) H44(1.0385) H76(0.8493) H47(1.1069) H46(1.1434)
 H45(1.1151) H11A(0.1621) H11B(0.2251) H11C(0.2104) H114(0.2492) H111(0.3761)
 H11G(0.2076) H11H(0.2771) H11I(0.2577) H11J(0.2633) H11K(0.1937) H11L(0.2222)
 H11M(0.392) H11N(0.439) H11O(0.3685) H12A(0.1486) H120(0.174) H117(0.6804)
 H11D(0.1368) H11E(0.1151) H11F(0.1828) H123(0.3076) H3VA(0.023) H3VB(0.0881)
 H3VC(0.0451) H10M(0.3913) H10N(0.4595) H10O(0.421) H12B(0.2538) H12C(0.1854)
 H12D(0.2312) H126(0.1496) H11P(0.7192) H11Q(0.7873) H11R(0.7363) H108(0.331)
 H10A(0.2677) H10B(0.2682) H10C(0.2193) H12H(0.085) H12I(0.0287) H12J(0.0938)
 H12K(0.0221) H12L(0.0111) H12M(0.0602) H11S(0.8239) H11T(0.8529) H11U(0.8116)
 H10D(0.3273) H10E(0.353) H10F(0.3827) H1A(0.0244) H12E(0.1967) H12F(0.1655)
 H12G(0.2223) H105(0.612) H142(0.4868) H10G(0.5209) H10H(0.5742) H10I(0.5318)
 H10J(0.6404) H10K(0.6718) H10L(0.6739) H14A(0.5924) H14B(0.6386) H14C(0.5841)
 H14D(0.5409) H14E(0.6036) H14F(0.5982)
;