Structure and Reactivity of Neutral and Cationictrans-N,N′-Dibenzylcyclam Zirconium Alkyl Complexes
Munhá, Rui F.; Antunes, M. Augusta; Alves, Luis G.; Veiros, Luis F.; Fryzuk, Michael D.; Martins, Ana M.; Organometallics 29 (2010) 3753–; doi:10.1021/om100465d

data_4066451
_publ_section_title
;
 Structure and Reactivity of Neutral and
 Cationictrans-N,N&#x2032;-Dibenzylcyclam Zirconium Alkyl Complexes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              3753
_journal_paper_doi               10.1021/om100465d
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C32 H52 N4 Zr, 0.5(C4 H10 O)'
_chemical_formula_sum            'C34 H57 N4 O0.5 Zr'
_chemical_formula_weight         621.05
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   34.251(8)
_cell_length_b                   43.849(9)
_cell_length_c                   8.9793(18)
_cell_measurement_reflns_used    2929
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      17.82
_cell_measurement_theta_min      2.39
_cell_volume                     13486(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    Sir97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0932
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       53
_diffrn_reflns_limit_k_min       -53
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            28341
_diffrn_reflns_theta_full        25.71
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         2.38
_exptl_absorpt_coefficient_mu    0.355
_exptl_absorpt_correction_T_max  0.9654
_exptl_absorpt_correction_T_min  0.9324
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5328
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.091
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     357
_refine_ls_number_reflns         6239
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0507
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1165
_reflns_number_gt                4692
_reflns_number_total             6239
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om100465d_si_002.cif
_cod_data_source_block           rmd83ortof
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/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_values 1715 2011-07-08 13:25:40Z adriana 

2021-10-24
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C68 H114 N8 O Zr2'
_cod_original_formula_weight         1242.11
_cod_original_formula_moiety         '2(C32 H52 N4 Zr), C4 H10 O'
_cod_original_formula_units_Z            8
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               4066451