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_1556524
_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
'C7 N7 Re, 2(C18 H22 Mn N2 O6), C24 H20 P, 6(O)'
_chemical_formula_sum            'C67 H64 Mn2 N11 O18 P Re'
_chemical_formula_weight         1638.34
_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
_atom_sites_solution_primary     dual
_cell_angle_alpha                84.638(3)
_cell_angle_beta                 82.694(4)
_cell_angle_gamma                65.057(3)
_cell_formula_units_Z            2
_cell_length_a                   14.2002(9)
_cell_length_b                   15.7993(9)
_cell_length_c                   18.0470(11)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.83
_cell_measurement_theta_min      2.62
_cell_volume                     3637.9(4)
_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 0.995
_diffrn_measured_fraction_theta_max 0.985
_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  0.0281
_diffrn_reflns_av_unetI/netI     0.0426
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43543
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.881
_diffrn_reflns_theta_min         1.589
_exptl_absorpt_coefficient_mu    2.098
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5533
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_density_meas      .
_exptl_crystal_description       prism
_exptl_crystal_F_000             1654
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.182
_refine_diff_density_min         -0.784
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     909
_refine_ls_number_reflns         18851
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0394
_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^)+(0.0310P)^2^+7.9890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.0978
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                16297
_reflns_number_total             18851
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cd3_kv883.cif
_cod_data_source_block           kv883
_cod_database_code               1556524
_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.a Rotating group:
 O23(H23A,H23B), O24(H24A,H24B), O13(H13A,H13B), O14(H14A,H14B)
2.b Secondary CH2 refined with riding coordinates:
 C217(H21A,H21B), C218(H21C,H21D), C117(H11A,H11B), C118(H11C,H11D)
2.c Aromatic/amide H refined with riding coordinates:
 C212(H212), C213(H213), C214(H214), C216(H216), C219(H219), C223(H223),
 C224(H224), C225(H225), C112(H112), C113(H113), C114(H114), C116(H116),
 C119(H119), C123(H123), C124(H124), C125(H125), C42(H42), C43(H43), C44(H44),
 C45(H45), C46(H46), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62),
  C63(H63), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73), C74(H74),
 C75(H75), C76(H76)
2.d Idealised Me refined as rotating group:
 C226(H22A,H22B,H22C), C227(H22D,H22E,H22F), C126(H12A,H12B,H12C), C127(H12D,
 H12E,H12F)
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_olex2_submission_special_instructions 'No special instructions were received'