A route to small clusters: a twisted half-hexagram-shaped M4(OH)4 cluster and its capacity for hosting closed-shell metals
Ara, I.; García-Monforte, M. A.; González, R.; Falvello, L. R.; Tomás, M.; Chemical Communications  (2017) –; doi:10.1039/C7CC07712B

data_7120881
_publ_section_title
;
 A route to small clusters: a twisted half-hexagram-shaped M4(OH)4 cluster
 and its capacity for hosting closed-shell metals
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC07712B
_journal_year                    2017
_chemical_formula_moiety
;
(C16 H36 N 1+)2, C48 H4 Cl40 O4 Pt4, 2(C3 H6 O)
;
_chemical_formula_sum            'C86 H88 Cl40 N2 O6 Pt4'
_chemical_formula_weight         3443.94
_chemical_name_common            'Local reference Estr. 1039, "Pt4"'
_chemical_name_systematic        'compound 1'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-03-09 deposited with the CCDC.
2017-11-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   50.3157(9)
_cell_length_b                   13.2707(2)
_cell_length_c                   17.5344(2)
_cell_measurement_reflns_used    37443
_cell_measurement_temperature    173(1)
_cell_measurement_theta_max      30.1140
_cell_measurement_theta_min      4.2050
_cell_volume                     11708.1(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics
;
Diamond v3.2k
Brandenburg, K. (2006). <i>DIAMOND</i>. Crystal Impact GbR, Bonn, Germany. 
;
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution
;
SIR-92
Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C.,
Polidori, G. & Camalli, M. (1994). <i>J. Appl. Cryst.</i> <b>27</b>, 435.
;
_diffrn_ambient_temperature      173(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0464
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       65
_diffrn_reflns_limit_h_min       -61
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            76053
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        27.500
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         4.804
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.726
_exptl_absorpt_correction_T_max  0.703
_exptl_absorpt_correction_T_min  0.247
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Multi-scan absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.954
_exptl_crystal_description       needle
_exptl_crystal_F_000             6632
_exptl_crystal_size_max          0.424
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.065
_refine_diff_density_max         1.840
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Flack x determined using 10963 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0132(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1255
_refine_ls_number_reflns         26376
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0200P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0556
_refine_ls_wR_factor_ref         0.0567
_reflns_Friedel_coverage         0.909
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                25077
_reflns_number_total             26376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc07712b2.cif
_cod_data_source_block           1
_cod_database_code               7120881
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.195
_shelx_estimated_absorpt_t_max   0.707
_exptl_absorpt_special_details
; 
Both numerical and multi-scan corrections were applied.
;
_shelx_res_checksum              5211