The template synthesis of triaryl functionalised 1,5,9-triphosphacyclododecane on molybdenum using organocopper reagents †
Jones, David J.; Edwards, Peter G.; Tooze, Robert P.; Albers, Thomas; Journal of the Chemical Society, Dalton Transactions  (1999) 1045–; doi:10.1039/a900509i

data_7027271
_publ_section_title
;
 The template synthesis of triaryl functionalised
 1,5,9-triphosphacyclododecane on molybdenum using organocopper
 reagents&#x200A;&#x2020;
;
_journal_issue                   7
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1045
_journal_paper_doi               10.1039/a900509i
_journal_year                    1999
_chemical_formula_sum            'C30 H33 Mo O3 P3'
_chemical_formula_weight         630.41
_chemical_name_systematic
; 
 1,5,9-triphenyl-1,5,9-triphosphacyclododecane molybdenum tricarbonyl
 complex
;
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.15(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   9.399(4)
_cell_length_b                   17.59(3)
_cell_length_c                   34.22(2)
_cell_measurement_temperature    293(2)
_cell_volume                     5658(10)
_computing_cell_refinement       MADNES
_computing_data_collection       MADNES
_computing_data_reduction        ABSMAD
_computing_molecular_graphics    ZORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type
;
 CAD-4 equipped with FAST TV area detector
;
_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  0.0968
_diffrn_reflns_av_sigmaI/netI    0.1588
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            14926
_diffrn_reflns_theta_full        19.78
_diffrn_reflns_theta_max         19.78
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.481
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2592
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.805
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         5023
_refine_ls_number_restraints     859
_refine_ls_restrained_S_all      0.793
_refine_ls_R_factor_all          0.0833
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0077P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                3038
_reflns_number_total             5023
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            900509isup1.cif
_cod_data_source_block           98pge014
_cod_original_cell_volume        5656(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7027271