# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2011


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_coden_ASTM              ?
_journal_coeditor_code           ?
_journal_coeditor_name           ?
_journal_coeditor_notes          
; ?
;
_journal_date_accepted           ?
_journal_date_from_coeditor      ?
_journal_date_printers_final     ?
_journal_date_printers_first     ?
_journal_date_proofs_in          ?
_journal_date_proofs_out         ?

#==============================================================================
# 2. PROCESSING SUMMARY (IUCr Office Use Only)

_journal_date_recd_electronic    ?
_journal_date_to_coeditor        ?
_journal_issue                   ?
_journal_page_first              ?
_journal_page_last               ?
_journal_paper_category          ?
_journal_suppl_publ_number       ?
_journal_suppl_publ_pages        ?
_journal_techeditor_code         ?
_journal_techeditor_notes        
; ?
;
_journal_volume                  ?
_journal_year                    ?
loop_
_publ_author_name
_publ_author_address
'E.Quartapelle Procopio'
; Departamento de Qu mica Inorganica,
Universidad de Granada,
Av. Fuentenueva s/n, 18071 Granada - Spain.
;
S.Rojas
; Departamento de Qu mica Inorganica,
Universidad de Granada,
Av. Fuentenueva s/n, 18071 Granada - Spain.
;
N.Munoz
; Departamento de Qu mica Organica,
Universidad de Granada,
Av. Fuentenueva s/n, 18071 Granada - Spain.
;
S.Galli
; Dipartimento di Scienze Chimiche e Ambientali,
Universita degli Studi dell'Insubria,
Via Valleggio 11, 22100 Como - Italy.
;
N.Masciocchi
; Dipartimento di Scienze Chimiche e Ambientali,
Universita degli Studi dell'Insubria,
Via Valleggio 11, 22100 Como - Italy.
;
;
F.Linares
;
; Departamento de Qu mica Inorganica,
Universidad de Granada,
Av. Fuentenueva s/n, 18071 Granada - Spain.
;
D.Miguel
; Departamento de Qu mica Organica,
Universidad de Granada,
Av. Fuentenueva s/n, 18071 Granada - Spain.
;
E.J.Oltra
; Departamento de Qu mica Organica,
Universidad de Granada,
Av. Fuentenueva s/n, 18071 Granada - Spain.
;
J.A.R.Navarro
; Departamento de Qu mica Inorganica,
Universidad de Granada,
Av. Fuentenueva s/n, 18071 Granada - Spain.
;
E.Barea
; Departamento de Qu mica Inorganica,
Universidad de Granada,
Av. Fuentenueva s/n, 18071 Granada - Spain.
;
_publ_contact_author_address     
;
Dipartimento di Scienze Chimiche e Ambientali,
Universita degli Studi dell'Insubria,
Via Valleggio 11, 22100 Como - Italy.
;
_publ_contact_author_email       simona.galli@uninsubria.it
_publ_contact_author_fax         +39-031-2386630
_publ_contact_author_phone       +39-031-2386627

_publ_contact_author_name        'Dr. Simona Galli'
_publ_contact_letter             
;
;
_publ_requested_category         ?

#==============================================================================
# 3. TITLE AND AUTHOR LIST
_publ_section_title              
;
A Robust MOF for the controlled delivery
of the non conventional half-sandwich ruthenium(II) metallodrug RAPTA-C
;

data_1
_database_code_depnum_ccdc_archive 'CCDC 829304'
_iucr_compatibility_tag          ?

#==============================================================================
#data_Compound1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_structural     
'[Ni8 (O H)4 (H2 O)2 (C10 H4 N4)6] (H2 O)7 (C3 H7 N O)8'
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C84 H102 Ni8 N32 O21'
_chemical_formula_weight         2365.5
_chemical_melting_point          ?
_chemical_compound_source        synthesis

loop_
_atom_type_symbol
_atom_type_description
# _atom_type_scat_dispersion_real
# _atom_type_scat_dispersion_imag
_atom_type_scat_source

C C 'International Tables for Crystallography (Vol. IV)'
H H 'International Tables for Crystallography (Vol. IV)'
Ni Ni 'International Tables for Crystallography (Vol. IV)'
N N 'International Tables for Crystallography (Vol. IV)'
O O 'International Tables for Crystallography (Vol. IV)'

#==============================================================================
# 1.5. POWDER SPECIMEN AND CRYSTAL DATA
_space_group_crystal_system      cubic
_space_group_name_H-M_alt        Fm-3m
_space_group_name_Hall           ?
_symmetry_equiv_pos_as_xyz       '-x, -y, -z'
_cell_length_a                   26.49080(67)
_cell_length_b                   26.49080(67)
_cell_length_c                   26.49080(67)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18590.2(14)
_cell_formula_units_Z            4
_cell_measurement_temperature    298
_pd_calibration_special_details  
; ?
;
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    0.84
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4888

# The next three fields give the specimen dimensions in mm. The equatorial
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              20 # perpendicular to
# equatorial plane

_pd_spec_size_equat              10 # parallel to
# scattering vector
# in transmission
_pd_spec_size_thick              0.2 # parallel to
# scattering vector
# in reflection

# The next five fields are character fields that describe the specimen.
_pd_spec_mounting                
; packed powder pellet
;
_pd_spec_mount_mode              reflection # options are 'reflection'
# or 'transmission'
_pd_spec_shape                   flat_sheet # options are 'cylinder',
# 'flat_sheet' or 'irregular'

_pd_char_particle_morphology     plate-like
_pd_char_colour                  turquoise # use ICDD colour descriptions

# The next four fields are normally only needed for transmission experiments.
_exptl_absorpt_coefficient_mu    ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

#==============================================================================
# 1.6. EXPERIMENTAL DATA
_exptl_special_details           
; ?
;
# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_diffrn_ambient_temperature      298
_diffrn_source_target            Cu
_diffrn_source_type              'sealed X-ray tube'
_diffrn_measurement_device_type  'Bruker AXS D8 Advance'
_diffrn_detector_type            'Bruker Lynxeye linear PSD'
_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
; ?
;
# The following six items are used for angular dispersive measurements only.

loop_
_diffrn_radiation_type
'Cu K\a'
_diffrn_radiation_wavelength     CuK\a~1~
_diffrn_radiation_monochromator  'Nickel filter'

# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.

_pd_meas_number_of_points        5001
_pd_meas_2theta_range_min        5
_pd_meas_2theta_range_max        105
_pd_meas_2theta_range_inc        0.02

# The following three items are used for time-of-flight measurements only.
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/detc         ?
_pd_meas_2theta_fixed            ?

# The following fields are used to identify the programs used.
_computing_data_collection       ?
_computing_cell_refinement       'TOPAS-R 3.0 Bruker AXS 2005 Karlsruhe Germany'
_computing_data_reduction        ?
_computing_structure_solution    'TOPAS-R 3.0 Bruker AXS 2005 Karlsruhe Germany'
_computing_structure_refinement  'TOPAS-R 3.0 Bruker AXS 2005 Karlsruhe Germany'
_computing_molecular_graphics    ?
_computing_publication_material  'TOPAS-R 3.0 Bruker AXS 2005 Karlsruhe Germany'
#==============================================================================

# 1.7. REFINEMENT DATA
# Use the next field to give any special details about the fitting of the
# powder pattern.
_pd_proc_ls_special_details      
;
a. Despcription of the ligand

The use of a rigid body description for the crystallographic
independent portion of the 1,4-bispyrazolato-but-1,3-diyne ligand
does not allow the derivation of statistically meaningful
s.u.'s for its atoms, described by:
c1 ux=r1*0.5; uy 0 uz 0
c2 ux=r1*0.5+r2; uy 0 uz 0
c3 ux=r1*0.5+r2+r3; uy 0 uz 0
c4 ux=r1*0.5+r2+r3+r4*Cos(Deg 54); uy=r4*Sin(Deg 54); uz 0
h4 ux=r1*0.5+r2+r3+r4*Cos(Deg 54)+r5*Cos(Deg 108); uy=r4*Sin(Deg
54)+r5*Sin(Deg 108); uz 0
n1 ux=r1*0.5+r2+r3+r4*Cos(Deg 54)+r4*Cos(Deg 18); uy=r4*Sin(Deg
54)-r4*Sin(Deg 18); uz 0
prm !r1 1.39
prm !r2 1.25
prm !r3 1.39
prm !r4 1.36
prm !r5 0.95

with the following translations and rotations for its centre of mass
Translate(0.25, 0.25, 0)
Rotate_about_axies(0, 0, 45)

and with the following torsion angle
Rotate_about_points (90, C2, C3, "C4 H4 N1")

b. Description of the solvent

The difference Fourier map calculated with the Fcs of the framework alone
revealed that the solvent is highly disordered. Its electronic density
was modeled by locating, within the cavities, the number of dummy oxygen
atoms (O2-O6 in the following atom list) whose refined site occupation
factors, combined with the site multiplicity, represented the total
electron density of the solvent, as estimated from the elemental and TG
analyses. The presence of disorder was taken into account by assigning
to the dummy atoms a high isotropic thermal parameter, corresponding
to a mean displacement of 0.9 .
;

# The next three items are given as text
_pd_proc_ls_profile_function     'fundamental parameters approach'
_pd_proc_ls_background_function  'Chebychev polynomial'
_pd_proc_ls_pref_orient_corr     ?
_pd_proc_ls_prof_R_factor        0.016
_pd_proc_ls_prof_wR_factor       0.022
_pd_proc_ls_prof_wR_expected     0.009
_refine_special_details          
; ?
;
_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      1/[Y~i~]
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     47
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
# The following item is 'CHI squared'
_refine_ls_goodness_of_fit_all   ?

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          .01
_refine_ls_shift/su_mean         ?

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.
_pd_proc_2theta_range_min        5
_pd_proc_2theta_range_max        105
_pd_proc_2theta_range_inc        0.02

loop_
_pd_proc_wavelength
1.540562
1.544390

_pd_block_diffractogram_id       ? # The id used for the block
# containing the powder
# pattern profile (section 11).

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

#==============================================================================

# 1.8. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv

Ni Ni 32 0.05332(12) 0.05332(12) 0.05332(12) 1 1.71(12)
O1 O 24 0.0915(10) 0 0 1 3.71(12)
H1 H 24 0.1275 0 0 1 3.71(12)
C1 C 48 0.2685513 0.2685513 0 1 3.71(12)
C2 C 48 0.301917 0.301917 0 1 3.71(12)
C3 C 48 0.3390196 0.3390196 0 1 3.71(12)
C4 C 96 0.3603573 0.3603573 0.04153378 1 3.71(12)
H4 H 96 0.3525213 0.3525213 0.0756401 1 3.71(12)
N1 N 96 0.3948824 0.3948824 0.02566929 1 3.71(12)
O2 O 4 0.5 0 0 1.988(77) 60.0(12)
O4 O 24 0 -0.24787(72) 0 2.336(25) 60.0(12)
O5 O 192 0 -0.2215(13) 0 0.3296(30) 60.0(12)
O6 O 192 -0.6423(11) -0.5914(15) 0.5608(14) 0.35205 60.0(12)