Reactivity Studies of a Zirconium Methylidene Complex: Group Transfer and Methylenation Reactions
Kurogi, Takashi; Kamitani, Masahiro; Manor, Brian C.; Carroll, Patrick J.; Mindiola, Daniel J.; Organometallics 36 (2016) 74–; doi:10.1021/acs.organomet.6b00594

data_4088977
_publ_section_title
;
 Reactivity Studies of a Zirconium Methylidene Complex: Group Transfer and
 Methylenation Reactions
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              74
_journal_paper_doi               10.1021/acs.organomet.6b00594
_journal_volume                  36
_journal_year                    2016
_chemical_formula_moiety         'C52 H69 N O2 P2 Zr, C5 H12'
_chemical_formula_sum            'C57 H81 N O2 P2 Zr'
_chemical_formula_weight         965.38
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-05-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.16 svn.r3265 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.3061(15)
_cell_length_b                   10.3460(5)
_cell_length_c                   16.5525(9)
_cell_measurement_reflns_used    9853
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.36
_cell_volume                     5361.2(5)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1057
_diffrn_reflns_av_unetI/netI     0.0906
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            61558
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.301
_exptl_absorpt_coefficient_mu    0.304
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6062
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.564
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 3363 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         12168
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0677P)^2^+0.7253P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1180
_refine_ls_wR_factor_ref         0.1343
_reflns_Friedel_coverage         0.908
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.975
_reflns_number_gt                8974
_reflns_number_total             12168
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00594_si_002.cif
_cod_data_source_block           UP9068
_cod_database_code               4088977
_shelx_res_checksum              97885
_shelx_hkl_checksum              23128
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'