Calcium-Catalyzed Intermolecular Hydrophosphination
Crimmin, Mark R.; Barrett, Anthony G. M.; Hill, Michael S.; Hitchcock, Peter B.; Procopiou, Panayiotis A.; Organometallics 26 (2007) 2953–; doi:10.1021/om070200k

data_4073260
_publ_section_title
;
 Calcium-Catalyzed Intermolecular Hydrophosphination
;
_journal_issue                   12
_journal_name_full               Organometallics
_journal_page_first              2953
_journal_paper_doi               10.1021/om070200k
_journal_volume                  26
_journal_year                    2007
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C45 H59 Ca N2 O P'
_chemical_formula_sum            'C45 H59 Ca N2 O P'
_chemical_formula_weight         714.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-03-07T10:43:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 112.043(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.7419(8)
_cell_length_b                   19.4591(7)
_cell_length_c                   24.6209(10)
_cell_measurement_reflns_used    75075
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      22.986
_cell_measurement_theta_min      3.395
_cell_measurement_wavelength     0.71073
_cell_volume                     8322.9(6)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      0.526148E-1
_diffrn_orient_matrix_UB_12      -0.20525E-2
_diffrn_orient_matrix_UB_13      -0.13652E-2
_diffrn_orient_matrix_UB_21      0.226915E-1
_diffrn_orient_matrix_UB_22      0.165684E-1
_diffrn_orient_matrix_UB_23      0.414374E-1
_diffrn_orient_matrix_UB_31      0.55135E-2
_diffrn_orient_matrix_UB_32      -0.486024E-1
_diffrn_orient_matrix_UB_33      0.141836E-1
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1263
_diffrn_reflns_av_unetI/netI     0.1792
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            46359
_diffrn_reflns_theta_full        22.96
_diffrn_reflns_theta_max         22.96
_diffrn_reflns_theta_min         3.4
_diffrn_source                   'Enraf Nonius FR590'
_exptl_absorpt_coefficient_mu    0.224
_exptl_absorpt_correction_T_max  0.9742
_exptl_absorpt_correction_T_min  0.8406
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.141
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.505
_refine_diff_density_min         -0.345
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1802
_refine_ls_number_reflns         22459
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.1997
_refine_ls_R_factor_gt           0.1079
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0748P)^2^+15.9423P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2021
_refine_ls_wR_factor_ref         0.2461
_reflns_number_gt                12585
_reflns_number_total             22459
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om070200k-file001.cif
_cod_data_source_block           mar806
_cod_database_code               4073260