Neutron diffraction studies of a four-coordinated hydride in near square-planar geometry.
Liao, Jian-Hong; Dhayal, Rajendra Singh; Wang, Xiaoping; Kahlal, Samia; Saillard, Jean-Yves; Liu, C. W.; Inorganic chemistry 53 (2014) 11140–11145; doi:10.1021/ic501747e

data_4341250
_publ_section_title
;
 Neutron diffraction studies of a four-coordinated hydride in near
 square-planar geometry.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11140
_journal_page_last               11145
_journal_paper_doi               10.1021/ic501747e
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C54 H137 Cu20 O18 P9 S18, 1.5(C6 H6)'
_chemical_formula_sum            'C63 H146 Cu20 O18 P9 S18'
_chemical_formula_weight         3318.72
_chemical_name_common            '[Cu~20~H~11~(S~2~P(O^i^Pr)~2~)~9~],1.5benzene'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.409(1)
_cell_angle_beta                 87.479(1)
_cell_angle_gamma                65.658(2)
_cell_formula_units_Z            2
_cell_length_a                   16.2820(4)
_cell_length_b                   16.6588(4)
_cell_length_c                   24.1228(6)
_cell_measurement_temperature    100(2)
_cell_volume                     5948.5(3)
_computing_cell_refinement       Mantid
_computing_data_collection       'SNS PyDas'
_computing_data_reduction        'Mantid and anvred2x'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.081
_diffrn_measured_fraction_theta_max 0.081
_diffrn_measurement_device_type  'TOPAZ 6-Li-glass area detectors at the SNS'
_diffrn_measurement_method       Laue
_diffrn_radiation_source         'Spallation Neutron Source at ORNL, USA'
_diffrn_radiation_type           neutron
_diffrn_radiation_wavelength     1.0
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1278
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            16014
_diffrn_reflns_theta_full        78.51
_diffrn_reflns_theta_max         78.51
_diffrn_reflns_theta_min         7.70
_exptl_absorpt_coefficient_mu    0.2935
_exptl_absorpt_correction_T_max  0.9426
_exptl_absorpt_correction_T_min  0.8450
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
The linear absorption coefficient is wavelength dependent
and it is calculated as:
          mu = 1.218 + 1.717 * lambda  [cm^-1^]
The value of 0.2935 (mm^-1^)given in _exptl_absorpt_coefficient_mu
is the value at 1 \%A
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.622
_refine_diff_density_min         -0.908
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.219
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1966
_refine_ls_number_reflns         16014
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0863
_refine_ls_R_factor_gt           0.0863
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+8.7890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1835
_refine_ls_wR_factor_ref         0.1835
_reflns_number_gt                16014
_reflns_number_total             16014
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic501747e_si_001.cif
_cod_data_source_block           cu20h11neutron
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4341250.cif.
;
_cod_database_code               4341250