Self-assembly of Thiolato-Bridged Manganese(I)-Based Metallarectangles: One-pot Synthesis and Structural Characterization.
Ashok Kumar, Chowan; Nagarajaprakash, R.; Ramakrishna, Buthanapalli; Manimaran, Bala; Inorganic chemistry 54 (2015) 8406–8414; doi:10.1021/acs.inorgchem.5b01118

data_4346258
_publ_section_title
;
 Self-assembly of Thiolato-Bridged Manganese(I)-Based Metallarectangles:
 One-pot Synthesis and Structural Characterization.
;
_journal_issue                   17
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8406
_journal_page_last               8414
_journal_paper_doi               10.1021/acs.inorgchem.5b01118
_journal_volume                  54
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C56 H36 Mn4 N4 O12 S4, 3(C16 H10)'
_chemical_formula_sum            'C104 H66 Mn4 N4 O12 S4'
_chemical_formula_weight         1911.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2c'
_space_group_name_H-M_alt        'P 1 1 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4720)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.6699(6)
_cell_length_b                   35.774(3)
_cell_length_c                   13.2056(9)
_cell_measurement_temperature    150(2)
_cell_volume                     5040.6(6)
_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_measured_fraction_theta_full 0.955
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0656
_diffrn_reflns_av_unetI/netI     0.1243
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_k_min       -45
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25955
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         3.63
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.631
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1956
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         3.082
_refine_diff_density_min         -2.277
_refine_diff_density_rms         0.185
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.365
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         17115
_refine_ls_number_restraints     1106
_refine_ls_restrained_S_all      1.355
_refine_ls_R_factor_all          0.1600
_refine_ls_R_factor_gt           0.1430
_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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3701
_refine_ls_wR_factor_ref         0.3963
_reflns_number_gt                13227
_reflns_number_total             17115
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5b01118_si_002.cif
_cod_data_source_block           3.pyrene
_cod_original_cell_volume        5040.7(7)
_cod_database_code               4346258
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H18(0.1) H21(0.029) H27(0.029) H28(0.029) H30(0.029) H35(0.029)
 H36(0.029) H38(0.029) H39(0.029) H40(0.029) H42(0.029) H43(0.165) H45(0.076)
 H47(0.059) H48(0.029) H50(0.085) H51(0.099) H53(0.029) H54(0.029) H55(0.029)
 H56(0.076) H58(0.074) H68(0.029) H71(0.092) H72(0.029) H25(0.208) H95(0.231)
 H78(0.186) H2I(0.177) H2O(0.17) H1V(0.153) H2A(0.168) H29(0.213) H22(0.195)
 H65(0.181) H2Q(0.1) H2R(0.1) H2S(0.1) H2U(0.1) H2V(0.1) H2X(0.1) H2Y(0.1)
 H2Z(0.1) H3A(0.1) H3B(0.1) H2(0.165) H3(0.165) H1(0.165) H6(0.165) H9(0.165)
 H11(0.165) H13(0.165) H14(0.165) H1A(0.165) H1M(0.165) H1C(0.14) H1F(0.14)
 H1K(0.14) H1O(0.14) H1U(0.14) H1Y(0.14) H1Z(0.14) H2C(0.14) H2L(0.14)
 H3H(0.14) H1D(0.029)
 Fixed X: H18(0.026) H21(0.4467) H27(0.4573) H28(0.3681) H30(0.3656)
 H35(0.0551) H36(0.1215) H38(0.1328) H39(0.4531) H40(0.1431) H42(0.353)
 H43(0.3775) H45(0.0418) H47(0.4499) H48(0.3539) H50(0.3856) H51(0.1352)
 H53(0.4578) H54(0.0509) H55(0.1927) H56(0.0303) H58(0.4634) H68(0.1357)
 H71(0.1062) H72(0.3022) H25(0.1231) H95(0.1225) H78(0.2936) H2I(0.4654)
 H2O(0.4661) H1V(0.3618) H2A(0.3503) H29(0.193) H22(0.0471) H65(0.0586) H2Q(-
 0.1848) H2R(-0.1875) H2S(-0.221) H2U(-0.2614) H2V(-0.2917) H2X(-0.3095) H2Y(-
 0.3067) H2Z(-0.2733) H3A(-0.233) H3B(-0.2026) H2(0.393) H3(0.2054) H1(0.0248)
 H6(-0.0843) H9(-0.0773) H11(0.0451) H13(0.2327) H14(0.4133) H1A(0.5224)
 H1M(0.5156) H1C(-0.1011) H1F(-0.2483) H1K(-0.2033) H1O(-0.0534) H1U(0.1371)
 H1Y(0.3512) H1Z(0.4984) H2C(0.4534) H2L(0.3035) H3H(0.113) H1D(0.0454)
 Fixed Y: H18(0.2213) H21(0.0332) H27(0.2213) H28(0.2216) H30(0.1595)
 H35(0.0336) H36(0.2214) H38(0.1577) H39(0.1578) H40(0.023) H42(0.0278)
 H43(0.28) H45(0.2799) H47(0.2786) H48(0.0764) H50(0.3434) H51(0.2772) H53(-
 0.0133) H54(-0.0166) H55(-0.0165) H56(0.3461) H58(0.3425) H68(0.0736)
 H71(0.344) H72(-0.0188) H25(0.4316) H95(0.4787) H78(0.5183) H2I(0.5108)
 H2O(0.4637) H1V(0.4279) H2A(0.4756) H29(0.5201) H22(0.517) H65(0.4693)
 H2Q(0.2556) H2R(0.3201) H2S(0.3493) H2U(0.3454) H2V(0.3105) H2X(0.2476)
 H2Y(0.1831) H2Z(0.1538) H3A(0.1578) H3B(0.1927) H2(0.1536) H3(0.1235)
 H1(0.1574) H6(0.2191) H9(0.2826) H11(0.342) H13(0.3721) H14(0.3383)
 H1A(0.2765) H1M(0.2131) H1C(0.1703) H1F(0.2132) H1K(0.2764) H1O(0.3291)
 H1U(0.3493) H1Y(0.3352) H1Z(0.2924) H2C(0.2292) H2L(0.1765) H3H(0.1563)
 H1D(0.1585)
 Fixed Z: H18(0.7058) H21(0.4274) H27(0.4584) H28(0.744) H30(0.7451)
 H35(0.7353) H36(0.4125) H38(0.4132) H39(0.4587) H40(0.1821) H42(0.9909)
 H43(0.7526) H45(0.7071) H47(0.4543) H48(0.8733) H50(0.7434) H51(0.4089)
 H53(0.3052) H54(0.8519) H55(0.9829) H56(0.698) H58(0.4548) H68(0.2944)
 H71(0.4143) H72(0.1859) H25(0.3101) H95(0.1892) H78(0.1741) H2I(0.2799)
 H2O(0.4007) H1V(0.8659) H2A(0.9846) H29(0.9733) H22(0.8433) H65(0.7246)
 H2Q(0.2651) H2R(0.2762) H2S(0.43) H2U(0.617) H2V(0.7584) H2X(0.8416)
 H2Y(0.8305) H2Z(0.6767) H3A(0.4897) H3B(0.3483) H2(0.9704) H3(0.9385)
 H1(0.9077) H6(0.8888) H9(0.8897) H11(0.9104) H13(0.9423) H14(0.9732)
 H1A(0.9921) H1M(0.991) H1C(0.1203) H1F(0.065) H1K(0.0639) H1O(0.0974)
 H1U(0.151) H1Y(0.2199) H1Z(0.2752) H2C(0.2764) H2L(0.2429) H3H(0.1892)
 H1D(0.6993)
;
_olex2_submission_special_instructions 'No special instructions were received'