Facile synthesis of a hexanuclear zinc-acetato-trimethylsilylphosphinidene cluster: a single-source precursor to Zn3P2 nanoparticles
Lee, Kyungseop; Huang, Yining; Corrigan, John F.; Chemical Communications  (2019) –; doi:10.1039/C9CC04879K

data_7124123
_publ_section_title
;
 Facile synthesis of a hexanuclear
 zinc-acetato-trimethylsilylphosphinidene cluster: a single-source
 precursor to Zn3P2 nanoparticles
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC04879K
_journal_year                    2019
_chemical_formula_sum            'C45 H73 N5 O8 P4 Si4 Zn6'
_chemical_formula_weight         1440.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-06-18 deposited with the CCDC.    2019-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.009(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.4627(12)
_cell_length_b                   20.1882(9)
_cell_length_c                   18.3640(9)
_cell_measurement_reflns_used    9833
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.69
_cell_volume                     8064.6(7)
_computing_cell_refinement       SAINT
_computing_data_collection       Apex3
_computing_data_reduction        SAINT
_computing_molecular_graphics    NRCVAX
_computing_publication_material  cif2tables.py
_computing_structure_refinement  SHELXL
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      110
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            'Bruker Apex2'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Kappa Axis Apex2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            112141
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.745
_diffrn_reflns_theta_min         2.597
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.932
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6447
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2952
_exptl_crystal_size_max          0.329
_exptl_crystal_size_mid          0.219
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         15371
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+11.5032P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11256
_reflns_number_total             15371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc04879k2.cif
_cod_data_source_block           b19194
_cod_database_code               7124123
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.569
_shelx_estimated_absorpt_t_max   0.785
_shelx_res_checksum              26339
_shelx_fab_checksum              8873