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_4085391
_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         'C54 H36 N3 O15 Re3 S3, C4.5 H6'
_chemical_formula_sum            'C58.5 H42 N3 O15 Re3 S3'
_chemical_formula_weight         1681.73
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-04-09
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.6581(2)
_cell_length_b                   35.7402(6)
_cell_length_c                   30.3489(5)
_cell_measurement_reflns_used    18890
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.2256
_cell_measurement_theta_min      2.9689
_cell_volume                     11560.6(3)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'OXFORD DIFFRACTION SUPER NOVA'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0847
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            71385
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'Micro-Focus (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.445
_exptl_absorpt_correction_T_max  0.3447
_exptl_absorpt_correction_T_min  0.2249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             6456
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         2.101
_refine_diff_density_min         -1.728
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     746
_refine_ls_number_reflns         10166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0429
_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^)+(0.0510P)^2^+67.0424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1052
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                8557
_reflns_number_total             10166
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501005n_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4085391--4085392.cif.'
_cod_original_formula_sum        'C58.50 H42 N3 O15 Re3 S3'
_cod_database_code               4085391
_olex2_refinement_description
;
1. Others
 Fixed Sof: H66A(0.5) H66B(0.5) H66C(0.5)
 Fixed U12: C333(0) C555(0) C666(0)
 Fixed U23: C333(0) C555(0) C666(0)
 Fixed Uiso: H10A(0.048) H10B(0.048) H12(0.055) H13(0.065) H14(0.064)
 H15(0.052) H16(0.049) H17A(0.041) H17B(0.041) H19(0.047) H20(0.058) H21(0.057)
 H22(0.051) H23(0.041) H24A(0.049) H24B(0.049) H26(0.051) H27(0.062) H28(0.063)
 H29(0.056) H30(0.051) H31(0.036) H32(0.038) H34(0.034) H35(0.032) H38(0.051)
 H40(0.043) H42(0.038) H45(0.039) H46(0.036) H48(0.04) H47(0.032) H49(0.069)
 H50(0.08) H52(0.066) H53(0.062) H11A(0.19) H11B(0.19) H11C(0.19) H333(0.061)
 H444(0.083) H66A(0.198) H66B(0.198) H66C(0.198)
 Fixed X: H10A(0.7573) H10B(0.7258) H12(0.6052) H13(0.3998) H14(0.2393)
 H15(0.2813) H16(0.4879) H17A(0.9993) H17B(0.9443) H19(1.1899) H20(1.3866)
 H21(1.4361) H22(1.2903) H23(1.0908) H24A(0.5303) H24B(0.4882) H26(0.671)
 H27(0.871) H28(1.0065) H29(0.9378) H30(0.7307) H31(0.4662) H32(0.3525)
 H34(0.609) H35(0.7132) H38(0.3451) H40(0.244) H42(0.4107) H45(0.3598)
 H46(0.3593) H48(0.3161) H47(0.3121) H49(1.0283) H50(0.9269) H52(0.6626)
 H53(0.754) H11A(-0.044) H11B(0.0036) H11C(0.1026) C333(0) H333(0) H444(0.0082)
 C555(0) C666(0) H66A(-0.004) H66B(-0.073) H66C(0.077)
 Fixed Y: H10A(0.9464) H10B(0.9717) H12(0.9504) H13(0.9601) H14(0.9651)
 H15(0.9626) H16(0.9544) H17A(0.8386) H17B(0.7975) H19(0.8092) H20(0.7824)
 H21(0.7627) H22(0.7702) H23(0.7935) H24A(0.4122) H24B(0.4376) H26(0.4787)
 H27(0.4744) H28(0.4276) H29(0.3838) H30(0.3858) H31(0.8702) H32(0.8511)
 H34(0.7704) H35(0.7902) H38(0.8111) H40(0.7226) H42(0.7047) H45(0.5983)
 H46(0.5334) H48(0.5432) H47(0.608) H49(0.84) H50(0.8059) H52(0.8859)
 H53(0.9119) H11A(0.676) H11B(0.7119) H11C(0.6817) H333(0.7118) H444(0.6127)
 H66A(0.5547) H66B(0.5547) H66C(0.5547)
 Fixed Z: H10A(0.0636) H10B(0.0215) H12(0.1194) H13(0.1423) H14(0.0917)
 H15(0.017) H16(-0.0075) H17A(0.0777) H17B(0.0711) H19(0.1063) H20(0.0912)
 H21(0.0194) H22(-0.0367) H23(-0.0216) H24A(-0.3219) H24B(-0.3628) H26(-0.3959)
 H27(-0.4253) H28(-0.4005) H29(-0.3488) H30(-0.3235) H31(-0.0172) H32(-0.0783)
 H34(-0.0997) H35(-0.0366) H38(-0.2241) H40(-0.301) H42(-0.1817) H45(-0.3422)
 H46(-0.3331) H48(-0.205) H47(-0.2106) H49(-0.0845) H50(-0.1459) H52(-0.148)
 H53(-0.0861) H11A(0.8525) H11B(0.8257) H11C(0.8433) C333(0.75) H333(0.75)
 H444(0.8161) C555(0.75) C666(0.75) H66A(0.7196) H66B(0.7664) H66C(0.764)
;