The crystal structure of poly[bis(N,N-dimethylformamide-κ1 O)(μ4- 2′,5,5′,5′′-tetracarboxy-[1,1′:4′,1′′-terphenyl]-3,3′′-dicarboxylato-κ4 O:O′:O′′:O′′′)manganese(II)] — N,N-dimethylformamide (1/2), C36H40N4O16Mn
Li, Guoqiang; Chen, Guo; Liu, Yanping; Wang, Gao; Liu, Liyu; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1015–1017; doi:10.1515/ncrs-2020-0118

data_8105364
_publ_section_title
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 The crystal structure of poly[bis(N,N-dimethylformamide-\k1 O)(\m4-
 2&#x2032;,5,5&#x2032;,5&#x2032;&#x2032;-tetracarboxy-[1,1&#x2032;:4&#x2032;,1&#x2032;&#x2032;-terphenyl]-3,3&#x2032;&#x2032;-dicarboxylato-\k4
 O:O&#x2032;:O&#x2032;&#x2032;:O&#x2032;&#x2032;&#x2032;)manganese(II)]
 --- N,N-dimethylformamide (1/2), C36H40N4O16Mn
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_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1015
_journal_page_last               1017
_journal_paper_doi               10.1515/ncrs-2020-0118
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         '0.5(C60 H52 Mn2 N4 O28), 2(C3 H7 N O)'
_chemical_formula_sum            'C36 H40 Mn N4 O16'
_chemical_formula_weight         839.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 112.641(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.5247(11)
_cell_length_b                   19.0823(19)
_cell_length_c                   10.5502(11)
_cell_measurement_reflns_used    2155
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      23.879
_cell_measurement_theta_min      2.348
_cell_volume                     1955.6(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      296.15
_diffrn_measured_fraction_theta_full 0.804
_diffrn_measured_fraction_theta_max 0.810
_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  0.0403
_diffrn_reflns_av_unetI/netI     0.0842
_diffrn_reflns_Laue_measured_fraction_full 0.804
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8312
_diffrn_reflns_point_group_measured_fraction_full 0.804
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         2.135
_exptl_absorpt_coefficient_mu    0.415
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_meas      .
_exptl_crystal_description       block
_exptl_crystal_F_000             874
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         3009
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0968P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1601
_refine_ls_wR_factor_ref         0.1741
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1925
_reflns_number_total             3009
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0118_suppl.cif
_cod_data_source_block           w
_cod_database_code               8105364
_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
2. Restrained distances
 C14-N1
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C14) \\sim Ueq, Uanis(C14A) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C15A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 N1, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1, C14, C14A, C15A, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O8A, O8, N2, C16, C17, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=1-FVAR(1)
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15D)=Sof(H15E)=Sof(H15F)=
 FVAR(1)
 Sof(H6)=Sof(O8)=Sof(H16A)=1-FVAR(2)
 Sof(H5)=Sof(O8A)=Sof(H16)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C6(H6A), C9(H9), C12(H12), C13(H13), C16(H16), C16(H16A)
6.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C15A(H15A,H15B,H15C), C15(H15D,
 H15E,H15F), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C)
6.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O5(H5), O6(H6)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'