Crystal structures of three complexes of zinc chloride with tri-<i>tert</i>-butylphosphane
Finke, Aaron D.; Gray, Danielle L.; Moore, Jeffrey S.; Acta Crystallographica Section E 72 (2016) 35–39; doi:10.1107/S2056989015023373

data_2241428
_publ_contact_author
;
Aaron D. Finke
;
_publ_section_title
;
 Crystal structures of three complexes of zinc chloride with
 tri-<i>tert</i>-butylphosphane
;
_journal_coeditor_code           PK2569
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              35
_journal_page_last               39
_journal_paper_doi               10.1107/S2056989015023373
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Zn Cl4 (C12 H27 P1)2]'
_chemical_formula_moiety         'C24 H54 Cl4 P2 Zn2'
_chemical_formula_sum            'C24 H54 Cl4 P2 Zn2'
_chemical_formula_weight         677.15
_chemical_name_systematic
;
Di-\m-chlorido-bis[chloridobis(tri-<i>tert</i>-butylphosphane)zinc]
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6408(16)
_cell_length_b                   12.9891(14)
_cell_length_c                   16.8190(18)
_cell_measurement_reflns_used    1388
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      18.94
_cell_measurement_theta_min      2.42
_cell_volume                     3198.5(6)
_computing_cell_refinement
;
SAINT (Bruker, 2005)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
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SAINT (Bruker, 2005)
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_computing_molecular_graphics
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<i>OLEX2</i> (Bourhis et al., 2015)
;
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<i>OLEX2</i> (Bourhis et al., 2015)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      193.15
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1687
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.412
_diffrn_reflns_theta_min         2.421
_exptl_absorpt_coefficient_mu    1.946
_exptl_absorpt_correction_T_max  0.9985
_exptl_absorpt_correction_T_min  0.8459
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.217
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.417
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2942
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1010
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+3.8822P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0797
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                1836
_reflns_number_total             2942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2569sup1.cif
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_cod_depositor_comments
;Adding full bibliography for 2241428--2241430.cif.

 Adding full bibliography for 2241428--2241430.cif.
;
_cod_database_code               2241428
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_shelx_estimated_absorpt_t_min   0.677
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_shelx_res_checksum              39006