Molybdenum(0), ruthenium(II), palladium(II), platinum(II), copper(I) and gold(I) complexes of a new methoxy functionalised bis(phosphino)amine: synthesis and structure
Gaw, Kirsty G.; Smith, Martin B.; Slawin, Alexandra M. Z.; New Journal of Chemistry 24 (2000) 429–; doi:10.1039/b001458n

data_7051286
_publ_section_title
;
 Molybdenum(0), ruthenium(II), palladium(II), platinum(II), copper(I)
 and gold(I) complexes of a new methoxy functionalised
 bis(phosphino)amine: synthesis and structure
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              429
_journal_paper_doi               10.1039/b001458n
_journal_volume                  24
_journal_year                    2000
_chemical_formula_analytical     'C32 H28.50 Cl4.50 N O P2 Pd'
_chemical_formula_moiety
'C31 H27 Cl2 N O P2 Pd.(C H Cl2)0.5(CH2Cl2)0.5'
_chemical_formula_structural     'C32 H28.50 Cl4.50 N O P2 Pd'
_chemical_formula_sum            'C32 H28.5 Cl4.5 N O P2 Pd'
_chemical_formula_weight         770.92
_chemical_melting_point          ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.5020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.8731(3)
_cell_length_b                   14.3704(3)
_cell_length_c                   21.5491(5)
_cell_measurement_reflns_used    132
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      168
_cell_measurement_theta_min      12
_cell_volume                     3636.33(15)
_computing_cell_refinement       SMART/SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       SMART
_diffrn_measurement_method       CCD
_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  0.0374
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            22016
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        -
_diffrn_standards_interval_count -
_diffrn_standards_interval_time  -
_diffrn_standards_number         -
_exptl_absorpt_coefficient_mu    0.954
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.832801
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    -
_exptl_crystal_description       prism
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          .31
_exptl_crystal_size_mid          .26
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.980
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.0000(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.849
_refine_ls_goodness_of_fit_obs   0.840
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         8501
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_restrained_S_obs      0.840
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_obs          0.0559
_refine_ls_shift/esd_max         2.204
_refine_ls_shift/esd_mean        0.107
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1412P)^2^+4.9978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2341
_refine_ls_wR_factor_obs         0.1564
_reflns_number_observed          5354
_reflns_number_total             8551
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b001458n.txt
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/adriana/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1555 2011-01-17 13:19:09Z saulius 

The following automatic conversions were performed:

'_chemical_melting_point' value '-' was changed to '?' - the value is
undefined or not given.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value '-' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1412P)^2^+4.9978P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1412P)^2^+4.9978P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C32 H28.50 Cl4.50 N O P2 Pd'
_cod_database_code               7051286