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_1556525
_publ_section_title
;
 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
'2(C118.5 H112 Mn6 N22.5 O14 Re1.5), 2(Cl0.25 O0.5), 1.5(Cl), F6 P, O'
_chemical_formula_sum            'C237 H224 Cl2 F6 Mn12 N45 O30 P Re3'
_chemical_formula_weight         5616.35
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                94.4470(10)
_cell_angle_beta                 93.2230(10)
_cell_angle_gamma                94.1440(10)
_cell_formula_units_Z            1
_cell_length_a                   13.8130(3)
_cell_length_b                   15.0609(3)
_cell_length_c                   30.1361(7)
_cell_measurement_reflns_used    5205
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.69
_cell_measurement_theta_min      2.37
_cell_volume                     6222.1(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0787
_diffrn_reflns_av_unetI/netI     0.1284
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            53423
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.083
_diffrn_reflns_theta_max         25.083
_diffrn_reflns_theta_min         1.667
_exptl_absorpt_coefficient_mu    2.143
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6450
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_meas      .
_exptl_crystal_description       plate
_exptl_crystal_F_000             2829
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.416
_refine_diff_density_min         -1.186
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1593
_refine_ls_number_reflns         22053
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1331
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                13745
_reflns_number_total             22053
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cd4_kv836.cif
_cod_data_source_block           kv836_1_kv
_cod_database_code               1556525
_olex2_refinement_description
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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
 C815-Re2
 2.1 with sigma of 0.02
 C810-Re2
 2.1 with sigma of 0.02
 N815-C815
 1.16 with sigma of 0.02
 C813-N813
 1.16 with sigma of 0.02
 Re2-C810 = Re2-C811 = Re2-C815 = Re2-C814 = Re2-C816
 2.1 with sigma of 0.02
 N811-C811 = N810-C810 = N814-C814 = N815-C815 = N813-C813 = N816-C816
 1.16 with sigma of 0.002
 C812-Re2
 2.1 with sigma of 0.02
 C812-N812
 1.16 with sigma of 0.002
 C811-N811
 1.16 with sigma of 0.02
 C810-N810
 1.16 with sigma of 0.02
 Re2-C813
 2.1 with sigma of 0.02
 Re2-N816
 3.25 with sigma of 0.04
 Re2-N815
 3.25 with sigma of 0.04
 Re2-N814
 3.25 with sigma of 0.04
 Re2-N811
 3.25 with sigma of 0.04
 Re2-N810
 3.25 with sigma of 0.04
 N812-Re2
 3.25 with sigma of 0.04
 N813-Re2
 3.25 with sigma of 0.04
3. Others
 Fixed Sof: C814(0.5) Re2(0.5) N810(0.5) N811(0.5) N812(0.5) N813(0.5)
 N814(0.5) N815(0.5) N816(0.5) C810(0.5) C811(0.5) C812(0.5) C813(0.5)
 C815(0.5) C816(0.5) Cl2(0.25) Cl3(0.25) O2S(0.5) Cl1(0.5) O1S(0.5)
4.a Rotating group:
 O53(H53A,H53B), O63(H63A,H63B)
4.b Secondary CH2 refined with riding coordinates:
 C118(H11A,H11B), C119(H11F,H11G), C218(H21F,H21G), C219(H21A,H21B), C318(H31F,
 H31G), C319(H31D,H31E), C418(H41F,H41G), C419(H41D,H41E), C518(H51A,H51B),
 C519(H51F,H51G), C618(H61A,H61B), C619(H61F,H61G)
4.c Aromatic/amide H refined with riding coordinates:
 C111(H111), C112(H112), C115(H115), C117(H117), C120(H120), C123(H123),
 C124(H124), C127(H127), C211(H211), C212(H212), C215(H215), C217(H217),
 C220(H220), C223(H223), C224(H224), C227(H227), C311(H311), C312(H312),
 C315(H315), C317(H317), C320(H320), C323(H323), C324(H324), C327(H327),
 C411(H411), C412(H412), C415(H415), C417(H417), C420(H420), C423(H423),
 C424(H424), C427(H427), C511(H511), C512(H512), C515(H515), C517(H517),
 C520(H520), C523(H523), C524(H524), C527(H527), C611(H611), C612(H612),
 C615(H615), C617(H617), C620(H620), C623(H623), C624(H624), C627(H627)
4.d Idealised Me refined as rotating group:
 C114(H11C,H11D,H11E), C126(H12A,H12B,H12C), C214(H21C,H21D,H21E), C226(H22A,
 H22B,H22C), C314(H31A,H31B,H31C), C326(H32A,H32B,H32C), C414(H41A,H41B,H41C),
 C426(H42A,H42B,H42C), C514(H51C,H51D,H51E), C526(H52A,H52B,H52C), C614(H61C,
 H61D,H61E), C626(H62A,H62B,H62C)
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_olex2_submission_special_instructions 'No special instructions were received'