Insertion of sodium phosphaethynolate, Na[OCP], into a zirconium-benzyne complex.
Kieser, Jerod M.; Gilliard, Jr, Robert J; Rheingold, Arnold L.; Grützmacher, Hansjörg; Protasiewicz, John D.; Chemical communications (Cambridge, England) 53 (2017) 5110–5112; doi:10.1039/c7cc01482a

data_7119997
_publ_section_title
;
 Insertion of sodium phosphaethynolate, Na[OCP], into a zirconium-benzyne
 complex.
;
_journal_issue                   37
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5110
_journal_page_last               5112
_journal_paper_doi               10.1039/c7cc01482a
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety         'C50 H60 Na2 O6 P2 Zr2, 2(C4 H8 O)'
_chemical_formula_sum            'C58 H76 Na2 O8 P2 Zr2'
_chemical_formula_weight         1191.54
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-02-08 deposited with the CCDC.
2017-03-08 downloaded from the CCDC.
;
_cell_angle_alpha                93.428(5)
_cell_angle_beta                 100.442(4)
_cell_angle_gamma                98.703(4)
_cell_formula_units_Z            2
_cell_length_a                   10.3925(15)
_cell_length_b                   16.372(2)
_cell_length_c                   16.948(3)
_cell_measurement_reflns_used    9965
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.57
_cell_measurement_theta_min      2.15
_cell_volume                     2791.9(7)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            43409
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.680
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  0.0926
_exptl_absorpt_correction_T_min  0.0666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.544
_refine_diff_density_min         -0.637
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     649
_refine_ls_number_reflns         9838
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0596
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+6.4241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7419
_reflns_number_total             9838
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc01482a2.cif
_cod_data_source_block           pro76_a
_cod_depositor_comments
;
Adding full bibliography for 7119997--7119998.cif.

2023-11-22
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C29 H38 Na O4 P Zr'
_cod_original_formula_weight         595.77
_cod_original_formula_moiety         '0.5(C50 H60 Na2 O6 P2 Zr2), C4 H8 O'
_cod_original_formula_units_Z            4
_cod_original_cell_volume        2792.0(7)
_cod_database_code               7119997
_shelx_estimated_absorpt_t_max   0.933
_shelx_estimated_absorpt_t_min   0.898
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C49(H49A,H49B), C25(H25A,H25B), C43(H43A,H43B), C19(H19A,
 H19B), C50(H50A,H50B), C24(H24A,H24B), C21(H21A,H21B), C22(H22A,H22B),
 C45(H45A,H45B), C51(H51A,H51B), C20(H20A,H20B), C48(H48A,H48B), C46(H46A,H46B),
  C44(H44A,H44B), C52(H52A,H52B), C23(H23A,H23B), C47(H47A,H47B), C54(H54A,
 H54B), C53(H53A,H53B), C57(H57A,H57B), C58(H58A,H58B), C56(H56A,H56B),
 C55(H55A,H55B)
2.b Aromatic/amide H refined with riding coordinates:
 C39(H39), C40(H40), C32(H32), C26(H26), C30(H30), C31(H31), C7(H7), C14(H14),
 C37(H37), C9(H9), C5(H5), C38(H38), C6(H6), C8(H8), C29(H29), C35(H35), C3(H3),
  C2(H2), C33(H33), C17(H17), C4(H4), C10(H10), C16(H16), C1(H1), C34(H34),
 C27(H27), C15(H15), C28(H28)
;
_shelx_res_checksum              27072
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'