Crystal structure of bis(μ3-methanolato-κ3 O:O:O)-bis(μ2-methanolato-κ2 O:O)-dimethanol-bis{6,6′-(1,3-dihydroxyl-2-acetylpropane-1,3-diyl)bis(2-chloro-4-bromophenolato)}tetramanganese(III) C40H40Br4Cl4Mn4O16
Zhao, Ji-Xing; Zhao, Li; Wang, Fei; An, Qin-Qin; Li, Peng-Peng; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 851–853; doi:10.1515/ncrs-2017-0002

data_8106700
_publ_section_title
;
 Crystal structure of bis(\m3-methanolato-\k3
 O:O:O)-bis(\m2-methanolato-\k2
 O:O)-dimethanol-bis{6,6&#x2032;-(1,3-dihydroxyl-2-acetylpropane-1,3-diyl)bis(2-chloro-4-bromophenolato)}tetramanganese(III)
 C40H40Br4Cl4Mn4O16
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              851
_journal_page_last               853
_journal_paper_doi               10.1515/ncrs-2017-0002
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C40 H40 Br4 Cl4 Mn4 O16'
_chemical_formula_sum            'C40 H40 Br4 Cl4 Mn4 O16'
_chemical_formula_weight         1457.92
_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     direct
_cell_angle_alpha                70.650(13)
_cell_angle_beta                 75.462(10)
_cell_angle_gamma                81.085(10)
_cell_formula_units_Z            1
_cell_length_a                   9.3724(9)
_cell_length_b                   11.7867(16)
_cell_length_c                   12.3994(18)
_cell_measurement_reflns_used    1251
_cell_measurement_temperature    294.06(10)
_cell_measurement_theta_max      23.4460
_cell_measurement_theta_min      3.6740
_cell_volume                     1247.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.06(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega    2.00   47.00   1.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479   57.0000   90.0000 30

  2 omega   38.00   89.00   1.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   57.0000  -30.0000 34

  3 omega   -7.00   24.50   1.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   77.0000 -180.0000 21

  4 omega  -48.00   30.00   1.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -57.0000 -180.0000 52

  5 omega  -19.00   62.00   1.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -99.0000  -90.0000 54

  6 omega  -18.00   63.00   1.5000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -99.0000   60.0000 54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0178236000
_diffrn_orient_matrix_UB_12      0.0342619000
_diffrn_orient_matrix_UB_13      0.0397180000
_diffrn_orient_matrix_UB_21      0.0571213000
_diffrn_orient_matrix_UB_22      -0.0336984000
_diffrn_orient_matrix_UB_23      0.0282483000
_diffrn_orient_matrix_UB_31      0.0506955000
_diffrn_orient_matrix_UB_32      0.0422355000
_diffrn_orient_matrix_UB_33      -0.0384350000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_unetI/netI     0.1143
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8276
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.021
_diffrn_reflns_theta_min         3.464
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.474
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89097
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.941
_exptl_crystal_description       block
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         4908
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.1218
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0256P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2854
_reflns_number_total             4908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0002_suppl.cif
_cod_data_source_block           1
_cod_database_code               8106700
_reflns_odcompleteness_completeness 99.61
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O6-H6
 0.85 with sigma of 0.01
 C18-H6
 1.902009 with sigma of 0.02
 Mn1-H6
 2.748281 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C11(H11)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C15(H15), C17(H17)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-12-01
_olex2_submission_special_instructions 'No special instructions were received'