Structural rearrangements induced by acid-base reactions in metal carbonyl clusters: the case of [H3-nCo15Pd9C3(CO)38](n-) (n = 0-3).
Ciabatti, Iacopo; Femoni, Cristina; Gaboardi, Mattia; Iapalucci, Maria Carmela; Longoni, Giuliano; Pontiroli, Daniele; Riccò, Mauro; Zacchini, Stefano; Dalton transactions (Cambridge, England : 2003) 43 (2014) 4388–4399; doi:10.1039/c3dt52527a

data_7028987
_publ_section_title
;
 Structural rearrangements induced by acid-base reactions in metal
 carbonyl clusters: the case of [H3-nCo15Pd9C3(CO)38](n-) (n = 0-3).
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4388
_journal_page_last               4399
_journal_paper_doi               10.1039/c3dt52527a
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C67 H46 Co15 N2 O38 Pd9'
_chemical_formula_weight         3328.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.0990(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8483(10)
_cell_length_b                   35.860(3)
_cell_length_c                   17.9822(13)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.7405
_cell_measurement_theta_min      2.2715
_cell_volume                     8279.6(11)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'SCHAKAL99 (Keller, 1999)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0772
_diffrn_reflns_av_unetI/netI     0.0619
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            78939
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    4.902
_exptl_absorpt_correction_T_max  0.6146
_exptl_absorpt_correction_T_min  0.5077
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 Data were corrected for Lorentz polarization and absorption
 effects (empirical absorption corrections SADABS).
 R(int) = 0.1087 (selected reflections only, before parameter refinement)
 R(int) = 0.0596 (selected reflections only, after parameter refinement)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6340
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         3.006
_refine_diff_density_min         -2.104
_refine_diff_density_rms         0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1107
_refine_ls_number_reflns         14607
_refine_ls_number_restraints     450
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0666
_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^)+(0.0925P)^2^+115.9864P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1680
_refine_ls_wR_factor_ref         0.1985
_reflns_number_gt                9476
_reflns_number_total             14607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52527a.txt
_cod_data_source_block           '[HCo15Pd9C3(CO)38]2-'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/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        8279.7(11)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7028987