Discovering the pivotal role of carbonate in the formation of a bis-phenolate supported Co15 cluster
Ross McLellan; Julien Reze; Stephanie M. Taylor; Ruaraidh D. McIntosh; Euan K. Brechin; Scott J. Dalgarno; Chem.Commun. 50 (2014) 2202–; doi:10.1039/c4cc00167b

data_7111996
_publ_section_title
;
 Discovering the pivotal role of carbonate in the formation of a
 bis-phenolate supported Co15 cluster
;
_journal_name_full               Chem.Commun.
_journal_page_first              2202
_journal_paper_doi               10.1039/c4cc00167b
_journal_volume                  50
_journal_year                    2014
_chemical_formula_sum            'C196.5 H284 Co15 N13 O61'
_chemical_formula_weight         4688.47
_chemical_name_common            Co15(bisphenolate)6(carbonate3)
_chemical_name_systematic
; 
 ? 
;
_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                85.462(2)
_cell_angle_beta                 71.615(2)
_cell_angle_gamma                64.348(2)
_cell_formula_units_Z            2
_cell_length_a                   20.8311(10)
_cell_length_b                   22.9871(11)
_cell_length_c                   29.1866(13)
_cell_measurement_reflns_used    9838
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.03
_cell_measurement_theta_min      2.36
_cell_volume                     11928.4(10)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'Apex II'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'XSeed (Barbour, 2001)'
_computing_publication_material  'local program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker X8 Apex II CCD Diffractometer'
_diffrn_measurement_method       '\f and \w 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  0.0480
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            114209
_diffrn_reflns_theta_full        22.72
_diffrn_reflns_theta_max         22.72
_diffrn_reflns_theta_min         0.98
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.7745
_exptl_absorpt_correction_T_min  0.6725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             4374
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_platon_squeeze_details
;
Squeeze indicates a very large solvent volume in the 
unit cell. As stated in the manuscript it was possible
to identify one MeOH and 5 DMF per asymmetric unit 
from the electron density map. The remaining density 
was too diffuse to readily identify solvent type. 
Elemental analysis on the identifiable solvent was 
consistent with the formula we used for our
calculations, accounting for 436 electrons in the unit
cell. We propose that additional solvent loss from the 
sample may be due to crystallisation with Et2O, the 
solvent used for vapour diffusion and crystal growth. 
This is also consistent with observations that PXRD 
does not match upon prolonged standing of ground 
crystalline material studied and the solvent dependent
nature of the crystals (that can be observed upon
grinding and standing).   
;
_refine_diff_density_max         1.552
_refine_diff_density_min         -1.377
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.481
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1816
_refine_ls_number_reflns         31699
_refine_ls_number_restraints     194
_refine_ls_restrained_S_all      1.494
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0895
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2377
_refine_ls_wR_factor_ref         0.2523
_reflns_number_gt                18732
_reflns_number_total             31699
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4cc00167b.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C196.50 H284 Co15 N13 O61'
_cod_database_code               7111996