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_2241430
_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          '(C12 H28 P) [Zn Cl3 (H2 O1)], C2 H4 Cl2'
_chemical_formula_moiety         'C12 H28 P +, Cl3 H2 O Zn -, C2 H4 Cl2'
_chemical_formula_sum            'C14 H34 Cl5 O P Zn'
_chemical_formula_weight         492.00
_chemical_name_systematic
;
Tri-<i>tert</i>-butylphosphonium aquatrichloridozincate 1,2-dichloroethane
monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 98.909(7)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   25.3722(5)
_cell_length_b                   8.5841(2)
_cell_length_c                   32.912(2)
_cell_measurement_reflns_used    2316
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      67.29
_cell_measurement_theta_min      23.07
_cell_volume                     7081.7(5)
_computing_cell_refinement
;
CrystalClear (Rigaku, 2010)
;
_computing_data_collection
;
CrystalClear (Rigaku, 2010)
;
_computing_data_reduction
;
CrystalClear (Rigaku, 2010)
;
_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      123.15
_diffrn_detector_area_resol_mean 22.2222
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'kappa-stage diffractometer'
_diffrn_measurement_device_type  'Rigaku CCD area-detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'focusing graphite'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0825
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            67698
_diffrn_reflns_theta_full        67.687
_diffrn_reflns_theta_max         63.691
_diffrn_reflns_theta_min         6.512
_exptl_absorpt_coefficient_mu    7.279
_exptl_absorpt_correction_T_max  0.8681
_exptl_absorpt_correction_T_min  0.3541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrystalClear; Rigaku, 2010)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.384
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.514
_refine_diff_density_min         -0.704
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         11604
_refine_ls_number_restraints     462
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0487
_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^)+(0.0718P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1241
_refine_ls_wR_factor_ref         0.1417
_reflns_number_gt                7131
_reflns_number_total             11604
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            pk2569sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;Adding full bibliography for 2241428--2241430.cif.

 Adding full bibliography for 2241428--2241430.cif.
;
_cod_original_cell_volume        7081.7(6)
_cod_database_code               2241430
_cod_database_fobs_code          2241430
_shelx_estimated_absorpt_t_min   0.354
_shelx_estimated_absorpt_t_max   0.868
_shelx_hkl_checksum              32374
_shelx_res_checksum              58464