Simple phosphinate ligands access zinc clusters identified in the synthesis of zinc oxide nanoparticles
Sebastian D. Pike; Edward R. White; Milo S. P. Shaffer; Charlotte K. Williams; Nature Communications 7 (2016) 13008–; doi:10.1038/ncomms13008

data_1548080
_publ_section_title
;
 Simple phosphinate ligands access zinc clusters identified in the
 synthesis of zinc oxide nanoparticles
;
_journal_name_full               'Nature Communications'
_journal_page_first              13008
_journal_paper_doi               10.1038/ncomms13008
_journal_volume                  7
_journal_year                    2016
_chemical_absolute_configuration .
_chemical_compound_source        'RCS1 312 Imperial College London'
_chemical_formula_moiety         'C56 H60 O8 P4 Zn4'
_chemical_formula_sum            'C56 H60 O8 P4 Zn4'
_chemical_formula_weight         1246.50
_chemical_melting_point          .
_chemical_name_systematic        Zn4Et4(DPPA)4
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-15
_audit_creation_method           CRYSTALS_ver_14.61
_cell_angle_alpha                90
_cell_angle_beta                 110.684(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.3886(5)
_cell_length_b                   10.1308(2)
_cell_length_c                   23.8034(5)
_cell_measurement_reflns_used    6282
_cell_measurement_temperature    173
_cell_measurement_theta_max      28
_cell_measurement_theta_min      3
_cell_volume                     5502.2(2)
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.025
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15051
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         26.369
_diffrn_reflns_theta_min         2.200
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.892
_exptl_absorpt_correction_T_max  0.80
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlisPro, (Agilent, 2011)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9733
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         5419
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.0022074
_refine_ls_shift/su_mean         0.0000445
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ +13.98P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0653
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_reflns_limit_h_max              28
_reflns_limit_h_min              -30
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              0
_reflns_number_gt                4663
_reflns_number_total             5438
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.43
_oxford_diffrn_Wilson_scale      0.72
_oxford_refine_ls_r_factor_ref   0.0374
_oxford_refine_ls_scale          1.242(3)
_oxford_reflns_number_all        5419
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title
'xcalibur in W:\Seb Pike\SC X-ra At 16:54 on '
_cod_data_source_file            ncomms13008-s3.cif
_cod_data_source_block           1A
_cod_original_cell_volume        5502.16(12)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               1548080