Reactions of metallated cyclohexyl phosphine (CyPHM) with As(NMe2)3; synthesis of [(CyP)4As]‒ anions (M = Li or Na, Cy = cyclohexyl)
Bashall, Alan; García, Felipe; Hopkins, Alexander A.; Wood, Jody A.; McPartlin, Mary; Woods, Anthony D.; Wright, Dominic S.; Dalton Transactions  (2003) 1143–; doi:10.1039/b211037g

data_7012460
_publ_section_title
;
 Reactions of metallated cyclohexyl phosphine (CyPHM) with As(NMe2)3;
 synthesis of [(CyP)4As]-- anions (M = Li or Na, Cy = cyclohexyl)
;
_journal_issue                   6
_journal_name_full               'Dalton Transactions'
_journal_page_first              1143
_journal_paper_doi               10.1039/b211037g
_journal_year                    2003
_chemical_formula_sum            'C30 H60 As N2 Na P4'
_chemical_formula_weight         670.59
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 92.037(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8971(3)
_cell_length_b                   17.5762(6)
_cell_length_c                   19.5359(7)
_cell_measurement_temperature    180(2)
_cell_volume                     3739.3(2)
_computing_cell_refinement       maXus
_computing_data_collection       maXus
_computing_data_reduction        maXus
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    teXsan
_diffrn_ambient_temperature      180(2)
_diffrn_measurement_device       NoniusKappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            18697
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.112
_exptl_absorpt_correction_T_max  1.078
_exptl_absorpt_correction_T_min  0.927
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements Sortav (Blessing 1995)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.191
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.022
_refine_ls_goodness_of_fit_obs   1.065
_refine_ls_matrix_type           full
_refine_ls_number_parameters     347
_refine_ls_number_reflns         6514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      2.192
_refine_ls_restrained_S_obs      1.065
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_obs          0.0387
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0003P)^2^+1.6959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1682
_refine_ls_wR_factor_obs         0.0706
_reflns_number_observed          4939
_reflns_number_total             6530
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b211037g.txt
_cod_data_source_block           dw0014
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'multiscan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0003P)^2^+1.6959P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0003P)^2^+1.6959P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7012460