# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_added_by_encifer
_database_code_depnum_ccdc_archive 'CCDC 1054571'
_audit_update_record             
;
2015-05-12 deposited with the CCDC.
2015-05-19 downloaded from the CCDC.
;
_iucr_compatibility_tag          ?

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

#data_Compound_CuBTPP

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_formula_moiety         'C42 H45 Cu3 N9 O5'
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_formula_iupac          ?
_chemical_formula_sum            'C42 H45 Cu3 N9 O5'
_chemical_formula_weight         946.46
_chemical_melting_point          ?
_chemical_compound_source        ?

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)'
Cu Cu '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      hexagonal
_space_group_name_H-M_alt        P6(3)/mmc
_space_group_name_Hall           ?

loop_
_symmetry_equiv_pos_as_xyz
'-x, -x+y, -z'
'-x, -x+y, z+1/2'
'-x, -y, -z'
'-x, -y, z+1/2'
'-x+y, -x, -z+1/2'
'-x+y, -x, z'
'-x+y, y, -z+1/2'
'-x+y, y, z'
'-y, -x, -z+1/2'
'-y, -x, z'
'-y, x-y, -z+1/2'
'-y, x-y, z'
'y, -x+y, -z'
'y, -x+y, z+1/2'
'y, x, -z'
'y, x, z+1/2'
'x-y, -y, -z'
'x-y, -y, z+1/2'
'x-y, x, -z'
'x-y, x, z+1/2'
'x, y, -z+1/2'
'x, y, z'
'x, x-y, -z+1/2'
'x, x-y, z'
_cell_length_a                   20.9247(95)
_cell_length_b                   20.9247(95)
_cell_length_c                   6.4
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     2426.8(22)
_cell_formula_units_Z            2
_cell_measurement_temperature    298

_pd_calibration_special_details  
; ?
;
_cell_special_details            
; ?
;

_exptl_crystal_density_diffrn    1.27
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             974

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              15 # perpendicular to 
# equatorial plane

_pd_spec_size_equat              20 # parallel to 
# scattering vector 
# in transmission

_pd_spec_size_thick              0.1 # 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     ?
_pd_char_colour                  'dark green' # 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        5051
_pd_meas_2theta_range_min        3
_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       'Bruker XRD Commander'
_computing_cell_refinement       TOPAS-R
_computing_data_reduction        ?
_computing_structure_solution    TOPAS-R
_computing_structure_refinement  TOPAS-R
_computing_molecular_graphics    ?
_computing_publication_material  ?

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

# 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      
; The use of a rigid body description for the crystallographically independent
  portion of the 1,3,5-tris((1H-pyrazol-4-ato)phenylene)benzene ligand
  did not allow the derivation of statistically meaningful s.u.s for its atoms.
  
  Its center of mass was located at (2/3, 1/3, 1/4) and the whole ligand
  was rotated by (90, 0, 60) with respect to the unit cell axis.
  
  The rigid body was described as follows:
  
  	z_matrix   H
	z_matrix   C1   H    =r1;
	z_matrix   C2   C1   =r1; H   60
	z_matrix   H2   C2   =r2; C1  120  H   180
	z_matrix   C3   C1   =r3; C2  120  H   180
	z_matrix   C4   C3   =r1; C1  120  C2  180
	z_matrix   H4   C4   =r2; C3  120  C1    0
	z_matrix   C5   C4   =r1; C3  120  C1  180
	z_matrix   H5   C5   =r2; C4  120  C3  180
	z_matrix   C6   C5   =r1; C4  120  C3    0
	z_matrix   C51  C6   =r1; C5  120  C4    0
	z_matrix   H51  C51  =r2; C6  120  C5  180
	z_matrix   C41  C51  =r1; C6  120  C5    0
	z_matrix   H41  C41  =r2; C51 120  C6  180
	z_matrix   C7   C6   =r3; C5  120  C4  180
	z_matrix   C8   C7   =r5; C6  126  C5    0
	z_matrix   H8   C8   =r2; C7  126  C6    0
	z_matrix   N1   C8   =r5; C7  108  C6  180
	z_matrix   N2   N1   =r5; C8  108  C7    0
	z_matrix   C9   N2   =r5; N1  108  C8    0
	z_matrix   H9   C9   =r2; N2  126  N1  180
	
	H = centre of mass
	prm r1 = 1.39 not refined
	prm r2 = 0.95 not refined
	prm r3 = 1.50 not refined
	prm r5 = 1.36 not refined
  
;

# 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        0.036
_pd_proc_ls_prof_wR_factor       0.048
_pd_proc_ls_prof_wR_expected     0.005

_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    fixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     25
_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        4
_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
Cu1 Cu 6 0.89286(44) -0.05357(22) 0.25 1 18.0(22)
O1 O 4 0 0 0.15 0.5 20.0(22)
O2 O 6 0.5 0 0.25 1 3
C1 C 6 0.7050193 0.2949807 0.25 1 20.0(22)
C2 C 6 0.7433719 0.3716859 0.25 1 20.0(22)
H2 H 6 0.7957963 0.3978982 0.25 1 20.0(22)
C3 C 6 0.746407 0.253593 0.25 1 20.0(22)
C4 C 12 0.7080544 0.1768878 0.25 1 20.0(22)
H4 H 12 0.6556299 0.1506756 0.25 1 20.0(22)
C5 C 12 0.746407 0.1385352 0.25 1 20.0(22)
H5 H 12 0.7201948 0.08611074 0.25 1 20.0(22)
C6 C 6 0.8231122 0.1768878 0.25 1 20.0(22)
C7 C 6 0.8644999 0.1355001 0.25 1 20.0(22)
C8 C 12 0.8339745 0.06086148 0.25 1 20.0(22)
H8 H 12 0.7826956 0.02578269 0.25 1 20.0(22)
N1 N 12 0.8897473 0.04525777 0.25 1 20.0(22)
