Larger pores and higher Tc: {[Ni(cyclam)]3[W(CN)8]2·solv}n‒ a new member of the largest family of pseudo-polymorphic isomers among octacyanometallate-based assemblies
Nowicka, Beata; Reczyński, Mateusz; Rams, Michał; Nitek, Wojciech; Kozieł, Marcin; Sieklucka, Barbara; CrystEngComm 17 (2015) 3526–; doi:10.1039/C5CE00287G

data_7220053
_publ_section_title
;
 Larger pores and higher Tc: {[Ni(cyclam)]3[W(CN)8]2&#x00B7;solv}n-- a new
 member of the largest family of pseudo-polymorphic isomers among
 octacyanometallate-based assemblies
;
_journal_issue                   18
_journal_name_full               CrystEngComm
_journal_page_first              3526
_journal_paper_doi               10.1039/C5CE00287G
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C48 H96 N28 Ni3 O10 W2'
_chemical_formula_sum            'C48 H96 N28 Ni3 O10 W2'
_chemical_formula_weight         1769.35
_chemical_name_systematic
'catena-(hexakis(?2-cyanido)-decacyanido-tris(1,4,8,11-tetraazacyclotetra  decane)-tri-nickel-di-tungsten solvate)'
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      12
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-03-18T11:27:58-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2015-03-19 deposited with the CCDC.
2015-04-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.772(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   32.105(5)
_cell_length_b                   15.068(5)
_cell_length_c                   9.331(5)
_cell_measurement_reflns_used    17706
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5855
_cell_measurement_theta_min      2.9808
_cell_volume                     4514(3)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
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        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
;
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3756
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0200486
_diffrn_orient_matrix_UB_12      -0.0133589
_diffrn_orient_matrix_UB_13      -0.0226396
_diffrn_orient_matrix_UB_21      0.0055584
_diffrn_orient_matrix_UB_22      -0.0105605
_diffrn_orient_matrix_UB_23      0.0718193
_diffrn_orient_matrix_UB_31      -0.0074384
_diffrn_orient_matrix_UB_32      -0.0438864
_diffrn_orient_matrix_UB_33      -0.0104017
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0343
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            31680
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_theta_full        25.24
_diffrn_reflns_theta_max         28.647
_diffrn_reflns_theta_min         3.179
_exptl_absorpt_coefficient_mu    3.208
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
        (compiled Aug  3 2011,13:03:54)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_description       plate
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
;
_refine_diff_density_max         1.389
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         5594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+3.5599P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                5043
_reflns_number_total             5594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00287g2.cif
_cod_data_source_block           bn_niwnic
_cod_depositor_comments          'Adding full bibliography for 7220053.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7220053
_shelx_estimated_absorpt_t_min   0.383
_shelx_estimated_absorpt_t_max   0.91
_shelxl_version_number           2012-9
_shelx_res_checksum              22335