Polycatenar pyrazole and pyrazolate ligands as building blocks of new columnar Pd(ii) metallomesogens.
Cuerva, Cristián; Campo, José A; Ovejero, Paloma; Torres, María R; Cano, Mercedes; Dalton transactions (Cambridge, England : 2003) 43 (2014) 8849–8860; doi:10.1039/c4dt00369a

data_7031271
_publ_section_title
;
 Polycatenar pyrazole and pyrazolate ligands as building blocks of new
 columnar Pd(ii) metallomesogens.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8849
_journal_page_last               8860
_journal_paper_doi               10.1039/c4dt00369a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C68 H100 N6 O4 Pd'
_chemical_formula_weight         1171.94
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                67.868(6)
_cell_angle_beta                 83.627(7)
_cell_angle_gamma                82.800(7)
_cell_formula_units_Z            1
_cell_length_a                   6.785(2)
_cell_length_b                   14.665(5)
_cell_length_c                   18.048(5)
_cell_measurement_reflns_used    678
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.30
_cell_measurement_theta_min      2.26
_cell_volume                     1646.4(9)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1462
_diffrn_reflns_av_sigmaI/netI    0.3901
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11266
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.22
_exptl_absorpt_coefficient_mu    0.331
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.851
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         5635
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      0.855
_refine_ls_R_factor_all          0.2632
_refine_ls_R_factor_gt           0.0717
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                1597
_reflns_number_total             5635
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt00369a2.cif
_cod_data_source_block           C68H100N6O4Pd1(2)in_the_manuscript
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1646.3(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7031271