Crystal structure of phosphonium carboxylate complexes. The role of the metal coordination geometry, ligand conformation and hydrogen bonding
Galkina, Irina; Tufatullin, Artem; Krivolapov, Dmitry; Bakhtiyarova, Yuliya; Chubukaeva, Dinara; Stakheev, Vitaly; Galkin, Vladimir; Cherkasov, Rafael; Büchner, Bernd; Kataeva, Olga; CrystEngComm 16 (2014) 9010–; doi:10.1039/C4CE01361A

data_7217269
_publ_section_title
;
 Crystal structure of phosphonium carboxylate complexes. The role of the
 metal coordination geometry, ligand conformation and hydrogen bonding
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              9010
_journal_paper_doi               10.1039/C4CE01361A
_journal_volume                  16
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C44 H42 Cl2 O4 P2 Zn, 2(H2 O)'
_chemical_formula_sum            'C44 H46 Cl2 O6 P2 Zn'
_chemical_formula_weight         869.02
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 98.154(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.129(3)
_cell_length_b                   12.883(2)
_cell_length_c                   18.871(3)
_cell_measurement_reflns_used    5236
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.42
_cell_measurement_theta_min      1.41
_cell_volume                     4362.9(12)
_computing_cell_refinement       'APEX2  v2, 1-4  (Bruker AXS, 2005-2007)'
_computing_data_collection       'APEX2  v2, 1-4  (Bruker AXS, 2005-2007)'
_computing_data_reduction        'SAINT NT v6.0 (Bruker AXS, 2003)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia, 1997), SCHAKAL (Keller, 1997)'
_computing_publication_material
'SHELXL97 (Sheldrick, 1997), WinGX (Farrugia 1999), enCIFer (Allen et al. 2004)'
_computing_structure_refinement
'SHELXL-97 (Sheldrick, 1997), WinGX (Farrugia 1999), PLATON (Spek 2005)'
_computing_structure_solution
'SHELXS-97 (Sheldrick, 2008), SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker SmartApex2'
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1104
_diffrn_reflns_av_sigmaI/netI    0.1921
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62162
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.804
_exptl_absorpt_correction_T_max  0.9534
_exptl_absorpt_correction_T_min  0.7830
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS version 2.10 (Sheldrick,Bruker AXS Inc.)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1808
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.072
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.144(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.829
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         19177
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      0.829
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1185
_refine_ls_wR_factor_ref         0.1443
_reflns_number_gt                7991
_reflns_number_total             19177
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ce01361a2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7217262--7217274.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7217269