Manganese- and Lanthanide-Based 1D Chiral Coordination Polymers as an Enantioselective Catalyst for Sulfoxidation.
Yadav, Munendra; Bhunia, Asamanjoy; Jana, Salil K.; Roesky, Peter W.; Inorganic chemistry 55 (2016) 2701–2708; doi:10.1021/acs.inorgchem.5b02234

data_4346850
_publ_section_title
;
 Manganese- and Lanthanide-Based 1D Chiral Coordination Polymers as an
 Enantioselective Catalyst for Sulfoxidation.
;
_journal_issue                   6
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2701
_journal_page_last               2708
_journal_paper_doi               10.1021/acs.inorgchem.5b02234
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C62 H82 Cl2 Mn2 N12 O26 Pr2, (H2O)'
_chemical_formula_sum            'C62 H84 Cl2 Mn2 N12 O27 Pr2'
_chemical_formula_weight         1891.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-04-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.88(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.726(7)
_cell_length_b                   10.721(2)
_cell_length_c                   25.497(5)
_cell_measurement_reflns_used    72916
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.21
_cell_measurement_theta_min      1.37
_cell_volume                     8116(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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      150.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0346
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            58171
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.772
_diffrn_reflns_theta_min         1.372
_exptl_absorpt_coefficient_mu    1.629
_exptl_absorpt_correction_T_max  0.8892
_exptl_absorpt_correction_T_min  0.7787
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   numerical
_exptl_crystal_colour            brownred
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       prism
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.141
_refine_diff_density_max         1.870
_refine_diff_density_min         -2.517
_refine_diff_density_rms         0.188
_refine_ls_abs_structure_details
;
 Flack x determined using 7396 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.077(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.255
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         17201
_refine_ls_number_restraints     59
_refine_ls_restrained_S_all      1.253
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+175.7091P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1896
_refine_ls_wR_factor_ref         0.1906
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.991
_reflns_number_gt                16536
_reflns_number_total             17201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic5b02234_si_002.cif
_cod_data_source_block           1
_cod_database_code               4346850
_shelxl_version_number           2013-2
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 O25B-C60B
 1.239 with sigma of 0.02
 C60B-N12B
 1.259 with sigma of 0.02
 N12B-C61B
 1.443 with sigma of 0.02
 N12B-C62B
 1.443 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C26: within 1.7A with sigma of 0.004 and sigma for terminal atoms of 0.008
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C48) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C48) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N11) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(C56)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: O14B(0.5) C46B(0.5) O21A(0.5) O22A(0.5) O25A(0.5) O26A(0.5)
 N9A(0.5) N12A(0.5) C51A(0.5) C52A(0.5) C53A(0.5) C60A(0.5) C61A(0.5) C62A(0.5)
 O21B(0.5) O25B(0.5) N12B(0.5) C52B(0.5) N9B(0.5) C60B(0.5) C61B(0.5) C62B(0.5)
 O27B(0.5) O27A(0.5) O26B(0.5) O22B(0.5) O14A(0.5) C0AA(0.5) C53B(0.5) C46A(0.5)
5.a Ternary CH refined with riding coordinates:
 C9(H9), C14(H14), C31(H31), C36(H36)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C13(H13A,H13B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C7(H7), C8(H8), C15(H15), C18(H18), C5AA(H5AA), C21(H21),
 C25(H25), C28(H28), C29(H29), C30(H30), C37(H37), C39(H39), C40(H40), C42(H42)
;
_shelx_res_checksum              1783
_shelx_hkl_checksum              53681
_olex2_submission_special_instructions 'No special instructions were received'