Oxime-Bridged Mn6 Clusters Inserted in One-Dimensional Coordination Polymer
Zaltariov, Mirela-Fernanda; Cazacu, Maria; Sacarescu, Liviu; Vlad, Angelica; Novitchi, Ghenadie; Train, Cyrille; Shova, Sergiu; Arion, Vladimir B.; Macromolecules 49 (2016) 6163–; doi:10.1021/acs.macromol.6b01149

data_1554166
_publ_section_title
;
 Oxime-Bridged Mn6 Clusters Inserted in One-Dimensional Coordination
 Polymer
;
_journal_issue                   17
_journal_name_full               Macromolecules
_journal_page_first              6163
_journal_paper_doi               10.1021/acs.macromol.6b01149
_journal_volume                  49
_journal_year                    2016
_chemical_formula_moiety
'C61 H67 Mn6 N7 O24 Si2, 1.2(H2 O), C7 H7 N O2'
_chemical_formula_sum            'C68 H76.4 Mn6 N8 O27.2 Si2'
_chemical_formula_weight         1826.79
_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     direct
_audit_creation_date             2016-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 105.62
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.029(5)
_cell_length_b                   25.005(5)
_cell_length_c                   19.750
_cell_measurement_reflns_used    483
_cell_measurement_temperature    244(60)
_cell_measurement_theta_max      29.4330
_cell_measurement_theta_min      2.2764
_cell_volume                     9050(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      244(60)
_diffrn_detector_area_resol_mean 8.0797
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega  -50.00    2.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2409  -57.0000   60.0000 52

  2 omega  -44.00   87.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2409    0.0000 -120.0000 131

  3 omega   64.00   89.00   1.0000  300.0000
omega____ theta____ kappa____ phi______ frames
    -       17.2409  178.0000 -150.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0327590000
_diffrn_orient_matrix_UB_12      -0.0151143000
_diffrn_orient_matrix_UB_13      -0.0085669000
_diffrn_orient_matrix_UB_21      -0.0069644000
_diffrn_orient_matrix_UB_22      0.0080130000
_diffrn_orient_matrix_UB_23      0.0320267000
_diffrn_orient_matrix_UB_31      -0.0194200000
_diffrn_orient_matrix_UB_32      0.0226174000
_diffrn_orient_matrix_UB_33      -0.0170849000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.2420
_diffrn_reflns_av_unetI/netI     0.2903
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16799
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        17.225
_diffrn_reflns_theta_max         17.225
_diffrn_reflns_theta_min         2.281
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.911
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
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    1.341
_exptl_crystal_description       prism
_exptl_crystal_F_000             3744
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.617
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     544
_refine_ls_number_reflns         5418
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.2381
_refine_ls_R_factor_gt           0.1067
_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^)+(0.1057P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2343
_refine_ls_wR_factor_ref         0.3069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2254
_reflns_number_total             5418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma6b01149_si_002.cif
_cod_data_source_block           shi_687_mz
_cod_original_formula_sum        'C68 H76.40 Mn6 N8 O27.20 Si2'
_cod_database_code               1554166
_chemical_oxdiff_formula         'C60 H60 N7 O18 Si2 Mn6'
_chemical_oxdiff_usercomment     H2_0809
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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) groups, All O(H,H) groups
2. Restrained distances
 O14-H14
 0.85 with sigma of 0.01
 N7-C49
 1.28 with sigma of 0.01
 O14-N7
 1.38 with sigma of 0.01
 N7-H14
 1.900728 with sigma of 0.02
 Mn5-H14
 3.150218 with sigma of 0.02
 O21-N8 \\sim O21X-N8
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(N6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O2) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uiso(C67) = Uiso(C62) = Uiso(C63) = Uiso(C64) = Uiso(C65) = Uiso(C66)
Uiso(O6W) = Uiso(O5W) = Uiso(O4W)
Uiso(O21) = Uiso(O21X)
4. Others
 Fixed Sof: O5W(0.4) H5WA(0.4) H5WB(0.4) O6W(0.4) H6WA(0.4) H6WB(0.4) O4W(0.4)
 H4WA(0.4) H4WB(0.4) O21(0.5) H21A(0.5) O21X(0.5) H21X(0.5)
 Fixed Uiso: O21(0.18484) O21X(0.18484)
5.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O14(H14), C54(H54A,H54B,H54C), C55(H55A,H55B,
 H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), O5W(H5WA,H5WB), O6W(H6WA,
 H6WB), O4W(H4WA,H4WB), O20(H20), O21(H21A), O21X(H21X)
5.b Rotating group:
 O3W(H3WA,H3WB)
5.c Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C58(H58A,H58B), C59(H59A,
 H59B), C60(H60A,H60B)
5.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C12(H12), C11(H11), C10(H10),
 C14(H14A), C19(H19), C16(H16), C17(H17), C18(H18), C21(H21), C25(H25),
 C24(H24), C23(H23), C26(H26), C28(H28), C33(H33), C32(H32), C31(H31), C30(H30),
  C35(H35), C39(H39), C38(H38), C37(H37), C40(H40), C42(H42), C45(H45),
 C46(H46), C47(H47), C44(H44), C49(H49), C64(H64), C63(H63), C66(H66), C65(H65),
  C68(H68)
5.e Fitted hexagon refined as free rotating group:
 C6(C1,C2,C3,C4,C5), C9(C8,C13,C12,C11,C10), C19(C20,C15,C16,C17,C18), C25(C24,
 C23,C22,C27,C26), C33(C32,C31,C30,C29,C34), C39(C38,C37,C36,C41,C40), C45(C46,
 C47,C48,C43,C44), C64(C63,C62,C67,C66,C65)
5.f Idealised tetrahedral OH refined as rotating group:
 O13(H13)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2011-11-19
_olex2_submission_special_instructions 'No special instructions were received'