Secondary diphosphine and diphosphido ligands: synthesis, characterisation and group 1 coordination compounds.
Ritch, Jamie S.; Julienne, Delphine; Rybchinski, Shayne R.; Brockman, Kathryne S.; Johnson, Kevin R. D.; Hayes, Paul G.; Dalton transactions (Cambridge, England : 2003) 43 (2014) 267–276; doi:10.1039/c3dt51844b

data_7029231
_publ_section_title
;
 Secondary diphosphine and diphosphido ligands: synthesis,
 characterisation and group 1 coordination compounds.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              267
_journal_page_last               276
_journal_paper_doi               10.1039/c3dt51844b
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C84 H136 K2 O16 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C92 H152 K2 O18 P2'
_chemical_formula_weight         1686.3456
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.891(2)
_cell_angle_beta                 87.743(2)
_cell_angle_gamma                68.936(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3096(19)
_cell_length_b                   17.990(3)
_cell_length_c                   21.542(3)
_cell_measurement_reflns_used    7013
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.68
_cell_measurement_theta_min      2.22
_cell_volume                     4808.2(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.0556
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            58552
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.194
_exptl_absorpt_correction_T_max  0.9907
_exptl_absorpt_correction_T_min  0.8866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.165
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.66
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.05
_platon_squeeze_details
;
The structure contained two severely disordered THF solvent molecules 
in the asymmetric unit, for which no suitable model could be found. The
electron density associated with the disordered regions was removed from
the reflection file using the SQUEEZE subroutine of PLATON, leaving a
void of ca. 645 A^3.

Accordingly, two THF molecules are included in _chemical_formula_moiety
(and _sum), and calculations of Mr, density, mu, and F(OOO) to more
accurately reflect the unit cell properties.
;
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.627
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1028
_refine_ls_number_reflns         16947
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1122
_refine_ls_R_factor_gt           0.0642
_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^)+(0.0957P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1805
_reflns_number_gt                10086
_reflns_number_total             16947
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt51844b.txt
_cod_data_source_block           complex7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/RSC/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 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        4808.3(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7029231