Insight into the stereoelectronic parameters of N-triphos ligands via coordination to tungsten(0).
Phanopoulos, Andreas; White, Andrew J. P.; Long, Nicholas J.; Miller, Philip W.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5536–5548; doi:10.1039/c6dt00170j

data_7038474
_publ_section_title
;
 Insight into the stereoelectronic parameters of N-triphos ligands via
 coordination to tungsten(0).
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5536
_journal_page_last               5548
_journal_paper_doi               10.1039/c6dt00170j
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C42 H37 N O3 P3 W, B F4, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C43.5 H40 B Cl3 F4 N O3 P3 W'
_chemical_formula_weight         1094.68
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL
_audit_update_record
;
2015-07-13 deposited with the CCDC.
2016-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.1122(4)
_cell_length_b                   35.0113(8)
_cell_length_c                   13.3447(3)
_cell_measurement_reflns_used    5760
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.3830
_cell_measurement_theta_min      2.8450
_cell_volume                     8462.3(3)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.822
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_av_unetI/netI     0.0810
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.822
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            18835
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.822
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.212
_diffrn_reflns_theta_min         2.577
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.093
_exptl_absorpt_correction_T_max  0.611
_exptl_absorpt_correction_T_min  0.494
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33a (release 28-03-2014 CrysAlis171 .NET)
(compiled Mar 28 2014,12:25:20)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.718
_exptl_crystal_description       blocks
_exptl_crystal_F_000             4344
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
 SQUEEZE suggested 498 e/cell = 62.3 e/asu
 The solvents used were ether (C4H10O, 42e), dcm (CH2Cl2, 42e),
 water (H2O, 10e) and methanol (CH4O, 18e).
 Before the use of SQUEEZE the solvent most resembled dcm.
 1.5CH2Cl2 = 63e, so this was used as the solvent present.
 
 So, the atom list is low by 1.5(CH2Cl2) = C1.5 H3 Cl3 and the UNIT is
 low by C12 H24 Cl24, i.e. C336 H296 B8 N8 O24 F32 P24 W8 Cl0
 
 The missing 5 non-H atoms would have required 45 variables (5 x 9)
 if refined anisotropically.
 The L.S. instruction was adjusted appropriately.
;
_refine_diff_density_max         1.729
_refine_diff_density_min         -5.917
_refine_diff_density_rms         0.203
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     510
_refine_ls_number_reflns         8710
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0761
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+210.7588P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1602
_refine_ls_wR_factor_ref         0.1669
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6893
_reflns_number_total             8710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00170j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7038473--7038480.cif.'
_cod_original_formula_sum        'C43.50 H40 B Cl3 F4 N O3 P3 W'
_cod_database_code               7038474
_shelxl_version_number           2013-4