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_2241429
_publ_section_title
;
 Crystal structures of three complexes of zinc chloride with
 tri-<i>tert</i>-butylphosphane
;
_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 Cl2 (C4 H8 O) (C12 H27 P)]'
_chemical_formula_moiety         'C16 H35 Cl2 O P Zn'
_chemical_formula_sum            'C16 H35 Cl2 O P Zn'
_chemical_formula_weight         410.68
_chemical_name_systematic
Dichlorido(tetrahydrofuran-\k<i>O</i>)(tri-<i>tert</i>-butylphosphane-\k<i>P</i>)zinc
_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
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.4580(11)
_cell_length_b                   8.9281(4)
_cell_length_c                   8.5790(4)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.75
_cell_volume                     2026.53(16)
_computing_cell_refinement
;
SAINT (Bruker, 2005)
;
_computing_data_collection
;
APEX2 (Bruker, 2004)
;
_computing_data_reduction
;
SAINT (Bruker, 2005), XPREP (Bruker, 2005), SADABS (Bruker,
2008) and
<i>TWINABS</i> (Bruker, 2008)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Bourhis et al., 2015)
;
_computing_publication_material
;
<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 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            23933
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.381
_diffrn_reflns_theta_min         2.408
_exptl_absorpt_coefficient_mu    1.552
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.5798
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.465
_exptl_crystal_size_mid          0.456
_exptl_crystal_size_min          0.266
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.304
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.206(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3698
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0318P)^2^+1.5653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                3581
_reflns_number_total             3698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2569sup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;Adding full bibliography for 2241428--2241430.cif.

 Adding full bibliography for 2241428--2241430.cif.
;
_cod_database_code               2241429
_cod_database_fobs_code          2241429
_shelx_hkl_checksum              23520
_shelx_res_checksum              78189