Tridentate phosphine ligands with novel linker-units
Findeis, Ralf A.; Gade, Lutz H.; Dalton Transactions  (2003) 249–; doi:10.1039/b209589k

data_7012277
_publ_section_title
;
 Tridentate phosphine ligands with novel linker-units
;
_journal_issue                   2
_journal_name_full               'Dalton Transactions'
_journal_page_first              249
_journal_paper_doi               10.1039/b209589k
_journal_year                    2003
_chemical_formula_moiety         'C50 H49 Mo O4 P3 Si'
_chemical_formula_sum            'C50 H49 Mo O4 P3 Si'
_chemical_formula_weight         930.89
_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'
_cell_angle_alpha                90
_cell_angle_beta                 97.864(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9160(2)
_cell_length_b                   22.8277(4)
_cell_length_c                   17.9896(4)
_cell_measurement_temperature    294
_cell_volume                     4440.62(16)
_computing_publication_material  CIFGEN_IN_OpenMoleN_(_1997)
_computing_structure_refinement  LSFM_OpenMoleN_(_1997)
_computing_structure_solution    Direct_methods_(SIR,_Burla_et_al.,_1989)
_diffrn_ambient_temperature      294
_diffrn_measurement_details
;
10365 reflections were collected using program Collect
("Collect" Data collection software, Nonius B.V., 1998)
The conditions were as follow : crystal to detector distance =  36. mm.
Scan angle =  1.4 deg 1 scans of   80 sec per frame.
Data collection was divided into  2 set(s)
with the following starting angles and number of frames :

Set 1 Theta =    6.30 Omega =    0.00 Kappa =    0.00  130 frames
Set 2 Theta =   -6.30 Kappa =  -86.00 Phi   =    0.00   34 frames
Friedel pairs were averaged. Internal R = 0.06
;
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       '\p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10365
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.475
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6225
_exptl_absorpt_correction_type   refdelf_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.39
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.479
_refine_diff_density_min         -0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   11.359
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6776
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.090
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.517
_refine_ls_wR_factor_ref         0.056
_reflns_number_gt                6776
_reflns_number_total             10365
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b209589k.txt
_cod_data_source_block           st882
_cod_original_cell_volume        4440.6(1)
_cod_database_code               7012277