#------------------------------------------------------------------------------
#$Date: 2017-05-18 04:16:46 +0300 (Thu, 18 May 2017) $
#$Revision: 196707 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/01/7120128.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7120128
loop_
_publ_author_name
'Helmdach, Kai'
'Ludwig, Stephan'
'Villinger, Alexander'
'Hollmann, Dirk'
'Kösters, Jutta'
'Seidel, Wolfram W.'
_publ_section_title
;
 Synthesis and activation potential of an open shell diphosphine.
;
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_paper_doi               10.1039/c7cc02114c
_journal_year                    2017
_chemical_formula_moiety         'C46 H48 B N7 O P2 W, 0.31(C H2 Cl2)'
_chemical_formula_sum            'C46.31 H48.62 B Cl0.62 N7 O P2 W'
_chemical_formula_weight         997.63
_chemical_name_systematic
'[(Carbonyl)(cyanido){bis(diphenylphosphino)acetylene}}{hydridotris(3,4,5-trimethylpyrazolyl)borate}tungsten(II)]'
_chemical_properties_physical
', Air-sensitive,Moisture-sensitive,Oxygen-sensitive'
_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   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-09-06 deposited with the CCDC.
2017-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.911(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.020(3)
_cell_length_b                   19.697(4)
_cell_length_c                   19.523(4)
_cell_measurement_reflns_used    9769
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.32
_cell_volume                     4970.4(18)
_computing_cell_refinement       'Bruker Apex V7.51A'
_computing_data_collection       'Bruker Apex V7.51A'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'ORTEP-3v2.01 (Farrugia, 1997)'
_computing_publication_material  SHELXL-2013
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 VENTURE diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1051
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            185332
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.999
_diffrn_reflns_theta_min         2.248
_exptl_absorpt_coefficient_mu    2.461
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2014)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_description       block
_exptl_crystal_F_000             2012
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane,n-pentane'
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.070
_platon_squeeze_details
;
The unit cell contains about 1.23 dichloromethane molecules which have been 
treated as a diffuse contribution to the overall scattering without specific 
atom positions by SQUEEZE/PLATON.
;
_refine_diff_density_max         3.380
_refine_diff_density_min         -4.860
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.228
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         13194
_refine_ls_number_restraints     678
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0693
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0066P)²+40.0014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1146
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11325
_reflns_number_total             13194
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7cc02114c2.cif
_cod_data_source_block           is_sl129b
_cod_original_cell_volume        4970.1(18)
_cod_database_code               7120128
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.556
_shelx_estimated_absorpt_t_max   0.847
_shelxl_version_number           2013-4
