Assembly of Mn(III) Schiff Base Complexes with Heptacyanorhenate (IV)
Sukhikh, T.S.; Vostrikova, K.E.; Inorganics 5 (2017) 59–; doi:10.3390/inorganics5030059

data_1556527
_publ_section_title
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 Assembly of Mn(III) Schiff Base Complexes with Heptacyanorhenate (IV)
;
_journal_name_full               Inorganics
_journal_page_first              59
_journal_paper_doi               10.3390/inorganics5030059
_journal_volume                  5
_journal_year                    2017
_chemical_formula_moiety
'C20 H23 Mn N3 O5, C18 H22 Mn N2 O6, 5(C2 H3 N), 2(C24 H20 B)'
_chemical_formula_sum            'C96 H100 B2 Mn2 N10 O11'
_chemical_formula_weight         1701.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 108.762(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.9891(18)
_cell_length_b                   27.544(3)
_cell_length_c                   21.779(2)
_cell_measurement_reflns_used    9604
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      20.00
_cell_measurement_theta_min      2.47
_cell_volume                     9081.9(17)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1043
_diffrn_reflns_av_unetI/netI     0.0741
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            125931
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.479
_exptl_absorpt_coefficient_mu    0.342
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6994
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0737 before and 0.0667 after correction. The Ratio of minimum to maximum transmission is 0.9384. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_density_meas      .
_exptl_crystal_description       needle
_exptl_crystal_F_000             3576
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.707
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         16018
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1189
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0650P)^2^+4.8480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1282
_refine_ls_wR_factor_ref         0.1556
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9349
_reflns_number_total             16018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cd6_kv908.cif
_cod_data_source_block           kv908
_cod_original_cell_volume        9081.7(17)
_cod_database_code               1556527
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 N51S-C52S = N71S_$1-C72S_$1
 1.12 with sigma of 0.002
 C53S-C52S = C72S_$1-C73S_$1
 1.45 with sigma of 0.002
 N61S-C62S
 1.12 with sigma of 0.002
 C62S-C63S
 1.45 with sigma of 0.002
 C73S-N71S
 2.55 with sigma of 0.04
 C53S-N51S
 2.55 with sigma of 0.04
 N61S-C63S
 2.55 with sigma of 0.004
3. Rigid bond restraints
 N11, N12, C128, C129
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uiso(N61S) = Uiso(N71S) = Uiso(C62S) = Uiso(C72S) = Uiso(C63S) = Uiso(C73S)
5. Others
 Sof(C117)=Sof(H11A)=Sof(H11B)=Sof(C118)=Sof(H11C)=Sof(H11D)=1-FVAR(1)
 Sof(C128)=Sof(H12G)=Sof(H12H)=Sof(C129)=Sof(H12I)=Sof(H12J)=FVAR(1)
 Fixed Sof: N51S(0.25) C52S(0.25) C53S(0.25) H53A(0.25) H53B(0.25) H53C(0.25)
 N71S(0.5) C72S(0.5) C73S(0.5) H73A(0.5) H73B(0.5) H73C(0.5) N61S(0.25)
 C62S(0.25) C63S(0.25) H63A(0.25) H63B(0.25) H63C(0.25)
6.a Rotating group:
 O13(H13A,H13B), O23(H23A,H23B), O24(H24A,H24B)
6.b Secondary CH2 refined with riding coordinates:
 C128(H12G,H12H), C129(H12I,H12J), C117(H11A,H11B), C118(H11C,H11D), C217(H21A,
 H21B), C218(H21C,H21D)
6.c Aromatic/amide H refined with riding coordinates:
 C112(H112), C113(H113), C114(H114), C116(H116), C119(H119), C123(H123),
 C124(H124), C125(H125), C212(H212), C213(H213), C214(H214), C216(H216),
 C219(H219), C223(H223), C224(H224), C225(H225), C311(H311), C312(H312),
 C313(H313), C314(H314), C315(H315), C317(H317), C318(H318), C319(H319),
 C320(H320), C321(H321), C323(H323), C324(H324), C325(H325), C326(H326),
 C327(H327), C329(H329), C330(H330), C331(H331), C332(H332), C333(H333),
 C411(H411), C412(H412), C413(H413), C414(H414), C415(H415), C417(H417),
 C418(H418), C419(H419), C420(H420), C421(H421), C423(H423), C424(H424),
 C425(H425), C426(H426), C427(H427), C429(H429), C430(H430), C431(H431),
 C432(H432), C433(H433)
6.d Idealised Me refined as rotating group:
 C126(H12A,H12B,H12C), C127(H12D,H12E,H12F), C131(H13C,H13D,H13E), C226(H22A,
 H22B,H22C), C227(H22D,H22E,H22F), C33S(H33A,H33B,H33C), C53S(H53A,H53B,H53C),
 C43S(H43A,H43B,H43C), C13S(H13F,H13G,H13H), C73S(H73A,H73B,H73C), C23S(H23C,
 H23D,H23E), C63S(H63A,H63B,H63C)
;
_olex2_submission_special_instructions 'No special instructions were received'