A new chiral metalladiphosphine for early‒late chemistry. Crystal structure of a D-camphor-based zirconium enolato phosphine and rearrangement of heterobimetallic Zr/Pd complexes †
Mattheis, Chris; Braunstein, Pierre; Fischer, Axel; Journal of the Chemical Society, Dalton Transactions  (2001) 800–; doi:10.1039/b008227i

data_7010360
_publ_section_title
;
 A new chiral metalladiphosphine for early--late chemistry. Crystal
 structure of a D-camphor-based zirconium enolato phosphine and
 rearrangement of heterobimetallic Zr/Pd complexes&#x200A;&#x2020;
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_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              800
_journal_paper_doi               10.1039/b008227i
_journal_year                    2001
_chemical_formula_moiety         'C48 H58 O4 P2 Pd'
_chemical_formula_sum            'C48 H58 O4 P2 Pd'
_chemical_formula_weight         867.34
_chemical_name_systematic        ' ?'
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_cell_angle_alpha                90
_cell_angle_beta                 112.670(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4840(2)
_cell_length_b                   34.0610(7)
_cell_length_c                   12.9620(2)
_cell_measurement_temperature    173
_cell_volume                     4271.06(17)
_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      173
_diffrn_measurement_details
;
180 frames, 60 sec/frame, delta phi = 1.0 deg. Each frame measured 2 times.
Detector to crystal distance 29 mm.
;
_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  0.039
_diffrn_reflns_av_sigmaI/netI    0.333
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            18151
_diffrn_reflns_theta_max         23.79
_diffrn_reflns_theta_min         2.5
_diffrn_source                   xray_tube
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.552
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.35
_exptl_crystal_density_method    none
_exptl_crystal_description       prism
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.081
_refine_ls_abs_structure_details 'Flack H D  (1983), Acta Cryst. A39,876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   6.686
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     990
_refine_ls_number_reflns         4817
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.037
_refine_ls_R_factor_gt           0.029
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 4Fo^2^/(\s^2^(Fo^2^) + 0.0009 Fo^4^)'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.222
_refine_ls_wR_factor_ref         0.035
_reflns_number_gt                4817
_reflns_number_total             5399
_reflns_threshold_expression     >3.0\s(I)
_cod_data_source_file            b008227i.txt
_cod_data_source_block           st338
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '4Fo^2^/(\s^2^(Fo^2^) + 0.0009
Fo^4^)' was changed to 'calc'. New tag '_refine_ls_weighting_details'
was created. The value of the new tag was set to 'w =
4Fo^2^/(\s^2^(Fo^2^) + 0.0009 Fo^4^)'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4271.1(3)
_cod_original_sg_symbol_Hall     ' P 2yb'
_cod_database_code               7010360