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_7045450
_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
'0.5(C70 H116 Cl6 Co2 N26 P8 Ru4), 2(C2 H6 O S)'
_chemical_formula_sum            'C39 H70 Cl3 Co N13 O2 P4 Ru2 S2'
_chemical_formula_weight         1308.50
_chemical_name_common            1DMSO
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-01-10
_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                 96.1210(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.4888(13)
_cell_length_b                   15.9993(12)
_cell_length_c                   17.5570(13)
_cell_measurement_reflns_used    6171
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.067
_cell_measurement_theta_min      2.216
_cell_volume                     5163.9(7)
_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      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0256
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16361
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.687
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.304
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0436 before and 0.0368 after correction. The Ratio of minimum to maximum transmission is 0.8805. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       prism
_exptl_crystal_F_000             2676
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.063
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         5452
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0248P)^2^+5.4852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0562
_refine_ls_wR_factor_ref         0.0581
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4912
_reflns_number_total             5452
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04515h2.cif
_cod_data_source_block           transRuRuCo-1DMSO
_cod_depositor_comments
'Adding full bibliography for 7045449--7045450.cif.'
_cod_database_code               7045450
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.797
_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. Shared sites
{C1P, N1P}
3. Uiso/Uaniso restraints and constraints
Uanis(C1P) = Uanis(N1P)
4. Others
 Fixed Sof: C1P(0.5) N1P(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C11(H11A,H11B), C16(H16A,H16B), C12(H12A,H12B), C13(H13A,
 H13B), C15(H15A,H15B), C25(H25A,H25B), C22(H22A,H22B), C23(H23A,H23B),
 C21(H21A,H21B), C26(H26A,H26B), C24(H24A,H24B)
5.b Aromatic/amide H refined with riding coordinates:
 C35(H35), C34(H34), C33(H33), C31(H31), C32(H32)
5.c Idealised Me refined as rotating group:
 C1D(H1DA,H1DB,H1DC), C2D(H2DA,H2DB,H2DC)
;
_olex2_submission_original_sample_id 1DMSO
_olex2_submission_special_instructions 'No special instructions were received'