Heterometallic 3d-4d coordination polymers assembled from trans-[Ru<sup>III</sup>(L)(CN)<sub>2</sub>]<sup>-</sup> tectons and 3d cations.
Marinescu, Gabriela; Madalan, Augustin M.; Maxim, Catalin; Shova, Sergiu; Clérac, Rodolphe; Andruh, Marius; Dalton transactions (Cambridge, England : 2003) 48 (2019) 15455–15464; doi:10.1039/c9dt01593k

data_1551223
_publ_section_title
;
 Heterometallic 3d-4d coordination polymers assembled from
 trans-[Ru<sup>III</sup>(L)(CN)<sub>2</sub>]<sup>-</sup> tectons and 3d
 cations.
;
_journal_issue                   41
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15455
_journal_page_last               15464
_journal_paper_doi               10.1039/c9dt01593k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety
'0.5(C220 H284 Co6 N52 O52 Ru8), 2(Cl O4), 4(C3 H7 N O)'
_chemical_formula_sum            'C122 H170 Cl2 Co3 N30 O38 Ru4'
_chemical_formula_weight         3316.84
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-05-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-15 deposited with the CCDC.    2019-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.638(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.2633(6)
_cell_length_b                   41.4370(10)
_cell_length_c                   13.5049(5)
_cell_measurement_reflns_used    8684
_cell_measurement_temperature    160.00(14)
_cell_measurement_theta_max      28.4720
_cell_measurement_theta_min      1.6230
_cell_volume                     7419.3(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      N~2~
_diffrn_ambient_temperature      160.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1593
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     -5.00  95.50   0.30   40.00    --   22.14  38.00 -60.00  335
  2  \w    -49.00  51.50   0.30   40.00    --   22.14 -38.00   0.00  335
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0254674000
_diffrn_orient_matrix_UB_12      0.0123716000
_diffrn_orient_matrix_UB_13      0.0361721000
_diffrn_orient_matrix_UB_21      -0.0469260000
_diffrn_orient_matrix_UB_22      0.0073190000
_diffrn_orient_matrix_UB_23      -0.0067571000
_diffrn_orient_matrix_UB_31      -0.0028843000
_diffrn_orient_matrix_UB_32      -0.0092909000
_diffrn_orient_matrix_UB_33      0.0429287000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0727
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            23688
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.536
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34717
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark brown'
_exptl_crystal_density_diffrn    1.485
_exptl_crystal_description       prism
_exptl_crystal_F_000             3414
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.241
_refine_diff_density_min         -1.420
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         13035
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0688
_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^)+(0.0822P)^2^+1.1429P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1641
_refine_ls_wR_factor_ref         0.1784
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10433
_reflns_number_total             13035
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01593k2.cif
_cod_data_source_block           shi_3173_maan
_cod_depositor_comments
'Adding full bibliography for 1551223--1551228.cif.'
_cod_database_code               1551223
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C30 H30 N6 O10 As1 Ru1 Co1'
_chemical_oxdiff_usercomment     Marinescu_7
_reflns_odcompleteness_completeness 98.93
_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
2. Restrained distances
 N8X-C25X = N8-C25
 1.48 with sigma of 0.01
 N7-C22X = N7B-C22
 1.48 with sigma of 0.01
 Co1-O7X \\sim Co1-O7
 with sigma of 0.01
 N6X-C28X \\sim N6-C28
 with sigma of 0.01
 O7X-C28X \\sim O7-C28
 with sigma of 0.01
 C27X-C25X \\sim C25X-C26X
 with sigma of 0.01
 C27-C25 \\sim C25-C26
 with sigma of 0.01
 N8X-C25 \\sim N8X-C25X
 with sigma of 0.01
 N8X-C26X \\sim N8-C26 \\sim N8X-C27X \\sim N8-C27
 with sigma of 0.01
 O5-C25X \\sim O5X-C25
 with sigma of 0.01
 C24X-C22 \\sim C22-C23X
 with sigma of 0.01
 C24-C22X \\sim C22X-C23
 with sigma of 0.01
 N7B-C22 \\sim N7B-C22X
 with sigma of 0.01
 N7-C23 \\sim N7B-C23X \\sim N7-C24 \\sim N7B-C24X
 with sigma of 0.01
 O6X-C22 \\sim O6-C22X
 with sigma of 0.01
 Co1-O6 \\sim Co1-O6X
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C30) = Uanis(C30X) = Uanis(C29) = Uanis(C29X)
Uanis(N6X) = Uanis(N6)
Uanis(O7) = Uanis(O7X)
Uanis(C28X) = Uanis(C28)
Uanis(O5) = Uanis(O5X) = Uanis(C25X) = Uanis(C25) = Uanis(N8X) = Uanis(C26X) =
Uanis(C26) = Uanis(C27X) = Uanis(N8) = Uanis(C27)
Uanis(O6) = Uanis(O6X) = Uanis(C22) = Uanis(C22X) = Uanis(N7) = Uanis(N7B) =
Uanis(C23) = Uanis(C23X) = Uanis(C24) = Uanis(C24X)
4. Others
 Sof(O7X)=Sof(N6X)=Sof(C28X)=Sof(H28X)=Sof(C29X)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30X)=Sof(H30A)=Sof(H30B)=Sof(H30C)=1-FVAR(1)
 Sof(O7)=Sof(N6)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29D)=Sof(H29E)=Sof(H29F)=
 Sof(C30)=Sof(H30D)=Sof(H30E)=Sof(H30F)=FVAR(1)
 Sof(O5X)=Sof(N8)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26D)=Sof(H26E)=Sof(H26F)=
 Sof(C27)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(2)
 Sof(O5)=Sof(N8X)=Sof(C25X)=Sof(H25X)=Sof(C26X)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27X)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(2)
 Sof(O6)=Sof(N7)=Sof(C22X)=Sof(H22X)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(H23C)=1-
 FVAR(3)
 Sof(O6X)=Sof(N7B)=Sof(C22)=Sof(H22)=Sof(C23X)=Sof(H23D)=Sof(H23E)=Sof(H23F)=
 FVAR(3)
 Fixed Sof: C24(0.5) H24A(0.5) H24B(0.5) H24C(0.5) C24X(0.5) H24D(0.5)
 H24E(0.5) H24F(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C10(H10A,H10B), C39(H39A,H39B), C40(H40A,H40B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C8(H8), C11(H11), C13(H13), C14(H14), C15(H15),
 C34(H34), C35(H35), C36(H36), C38(H38), C41(H41), C43(H43), C44(H44), C45(H45),
  C50(H50), C53(H53), C22X(H22X), C25X(H25X), C28X(H28X), C22(H22), C25(H25),
 C28(H28), C59(H59), C56(H56)
5.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C48(H48A,H48B,H48C), C49(H49A,H49B,
 H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C54(H54A,H54B,H54C), C55(H55A,
 H55B,H55C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26X(H26A,H26B,H26C),
 C27X(H27A,H27B,H27C), C29X(H29A,H29B,H29C), C30X(H30A,H30B,H30C), C23X(H23D,
 H23E,H23F), C24X(H24D,H24E,H24F), C26(H26D,H26E,H26F), C27(H27D,H27E,H27F),
 C29(H29D,H29E,H29F), C30(H30D,H30E,H30F), C60(H60A,H60B,H60C), C61(H61A,H61B,
 H61C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.686
_oxdiff_exptl_absorpt_empirical_full_min 0.619