Water driven formation of channels: unusual solid-state structural transformation of a heterometallic polymer.
Scalambra, Franco; Serrano-Ruiz, Manuel; Romerosa, Antonio; Dalton transactions (Cambridge, England : 2003) 47 (2018) 3588–3595; doi:10.1039/c7dt04515h

data_7045449
_publ_section_title
;
 Water driven formation of channels: unusual solid-state structural
 transformation of a heterometallic polymer.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3588
_journal_page_last               3595
_journal_paper_doi               10.1039/c7dt04515h
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'C70 H116 Cl6 Co2 N26 P8 Ru4, C35 H58 N13 P4 Ru2, 30(O), Cl'
_chemical_formula_sum            'C105 H234 Cl7 Co2 N39 O30 P12 Ru6'
_chemical_formula_weight         3867.37
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-01-11
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2017.12.08 svn.r3473 for OlexSys, GUI svn.r5433)
;
_audit_update_record
;
2018-01-18 deposited with the CCDC.
2018-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.6510(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7090(9)
_cell_length_b                   16.0946(12)
_cell_length_c                   44.352(3)
_cell_measurement_reflns_used    9883
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.84
_cell_measurement_theta_min      2.32
_cell_volume                     8354.7(11)
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            45999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.020
_diffrn_reflns_theta_min         1.564
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.020
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.7090
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0675 before and 0.0563 after correction. The Ratio of minimum to maximum transmission is 0.9508. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             3988
_exptl_crystal_size_max          0.051
_exptl_crystal_size_mid          0.019
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.608
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     949
_refine_ls_number_reflns         16422
_refine_ls_number_restraints     39
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0768
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0463P)^2^+49.4341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1420
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13516
_reflns_number_total             16422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04515h2.cif
_cod_data_source_block           cisRuRuCo-15H2O
_cod_depositor_comments
'Adding full bibliography for 7045449--7045450.cif.'
_cod_original_cell_volume        8354.8(11)
_cod_database_code               7045449
_shelx_shelxl_version_number     2018/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All H(H) groups, All C(H) groups, All C(H,H) groups
2. Shared sites
{CCN, NCN1}
{NCN, CCN1}
{CCNM, NCNM}
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(O5) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O6) \\sim
Ueq, Uanis(O4) \\sim Ueq, : with sigma of 0.1 and sigma for terminal atoms of
0.2
Uanis(CCN) = Uanis(NCN1)
Uanis(NCN) = Uanis(CCN1)
Uanis(CCNM) = Uanis(NCNM)
4. Others
 1*[Sof(O8)]+1*[Sof(O8A)]=1 with esd of 0.00001
 1*[Sof(O11)]+1*[Sof(O11C)]+1*[Sof(O11B)]+1*[Sof(O11A)]=1.5 with esd of 0.00001
 1*[Sof(O13B)]+1*[Sof(O13A)]=0.5 with esd of 0.00001
 1*[Sof(O12)]+1*[Sof(O13)]+1*[Sof(O12A)]=1 with esd of 0.00001
 1*[Sof(O9)]+1*[Sof(O9A)]=1 with esd of 0.00001
 1*[Sof(O14C)]+1*[Sof(O14D)]=0.5 with esd of 0.00001
 1*[Sof(O14E)]+1*[Sof(O14)]+1*[Sof(O14B)]=1 with esd of 0.00001
 1*[Sof(O15)]+1*[Sof(O15A)]=0.83 with esd of 0.00001
 1*[Sof(O10A)]+1*[Sof(O10)]=0.67 with esd of 0.00001
 Fixed Sof: NCN(0.5) CCN(0.5) CCNM(0.5) Cl4(0.5) CCN1(0.5) NCN1(0.5) NCNM(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C20(H20A,H20B), C4(H4A,H4B), C1(H1A,H1B), C28(H28A,H28B),
 C27(H27A,H27B), C26(H26A,H26B), C19(H19A,H19B), C24(H24A,H24B), C29(H29A,H29B),
  C23(H23A,H23B), C21(H21A,H21B), C5(H5A,H5B), C36(H36A,H36B), C18(H18A,H18B),
 C25(H25A,H25B), C7(H7A,H7B), C2(H2A,H2B), C8(H8A,H8B), C9(H9A,H9B), C41(H41A,
 H41B), C3(H3A,H3B), C35(H35A,H35B), C44(H44A,H44B), C12(H12A,H12B), C6(H6A,
 H6B), C42(H42A,H42B), C11(H11A,H11B), C37(H37A,H37B), C40(H40A,H40B), C10(H10A,
 H10B), C38(H38A,H38B), C43(H43A,H43B), C39(H39A,H39B), C46(H46A,H46B),
 C45(H45A,H45B)
5.b Aromatic/amide H refined with riding coordinates:
 C32(H32), C49(H49), C30(H30), C15(H15), C50(H50), C13(H13), C34(H34),
 C17(H17), C14(H14), C31(H31), C51(H51), C33(H33), C16(H16), C47(H47), C48(H48)
;
_olex2_submission_special_instructions 'No special instructions were received'