Poly[[tetra-μ-cyanido-κ^8^<i>C</i>:<i>N</i>-dodeca-cyanido-κ^12^<i>C</i>-tris(<i>N</i>,<i>N</i>-dimethylformamide-κ<i>O</i>)tris(methanol-κ<i>O</i>)tris(3,4,7,8-tetramethyl-1,10-phenanthroline-κ^2^<i>N</i>,<i>N</i>')trimanganese(II)ditungstate(V)] dihydrate]
Yang, Fei-Lin; Yang, Dan; Acta Crystallographica Section E 70 (2014) m170–m171; doi:10.1107/S1600536814007235

data_2239290
_publ_section_title
;
 Poly[[tetra-\m-cyanido-\k^8^<i>C</i>:<i>N</i>-dodeca-cyanido-\k^12^<i>C</i>-tris(<i>N</i>,<i>N</i>-dimethylformamide-\k<i>O</i>)tris(methanol-\k<i>O</i>)tris(3,4,7,8-tetramethyl-1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')trimanganese(II)ditungstate(V)]
 dihydrate]
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m170
_journal_page_last               m171
_journal_paper_doi               10.1107/S1600536814007235
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[Mn3 W2 (C N)16 (C16 H16 N2)3 (C3 H7 N O)3 (C H4 O)3], 2H2 O'
_chemical_formula_moiety         'C76 H81 Mn3 N25 O6 W2, 2(H2 O)'
_chemical_formula_sum            'C76 H85 Mn3 N25 O8 W2'
_chemical_formula_weight         2009.20
_chemical_name_systematic
'Poly[[tetra-\m-cyanido-\k^8^<i>C</i>:<i>N</i>-dodeca-cyanido-\k^12^<i>C</i>-tris(<i>N</i>,<i>N</i>-dimethylformamide-\k<i>O</i>)tris(methanol-\k<i>O</i>)tris(3,4,7,8-tetramethyl-1,10-phenanthroline-\k^2^<i>N</i>,<i>N</i>')trimanganese(II)ditungstate(V)] dihydrate]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                70.008(2)
_cell_angle_beta                 82.663(3)
_cell_angle_gamma                66.129(2)
_cell_formula_units_Z            2
_cell_length_a                   15.5038(17)
_cell_length_b                   16.4958(18)
_cell_length_c                   21.4067(13)
_cell_measurement_reflns_used    9991
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      27.26
_cell_measurement_theta_min      2.49
_cell_volume                     4704.4(8)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2013 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Bruker SMART APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0164
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35664
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         1.425
_exptl_absorpt_coefficient_mu    2.888
_exptl_absorpt_correction_T_max  0.60
_exptl_absorpt_correction_T_min  0.50
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.418
_exptl_crystal_description       block
_exptl_crystal_F_000             2006
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.382
_refine_diff_density_min         -0.917
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1078
_refine_ls_number_reflns         17934
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0461
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.07P)^2^+1.88P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1163
_refine_ls_wR_factor_ref         0.1167
_reflns_number_gt                14773
_reflns_number_total             17934
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz5113sup1.cf
_cod_data_source_block           I
_cod_database_code               2239290
_cod_database_fobs_code          2239290
_shelx_estimated_absorpt_t_min   0.544
_shelx_estimated_absorpt_t_max   0.624
_shelx_hkl_checksum              26017
_shelx_res_checksum              34535
_shelxl_version_number           20.13