Synthesis and structural studies of amido, hydrazido and imido zirconium(iv) complexes incorporating a diamido/diamine cyclam-based ligand
Munhá, Rui F.; Veiros, Luis F.; Duarte, M. Teresa; Fryzuk, Michael D.; Martins, Ana M.; Dalton Transactions  (2009) 7494–7508; doi:10.1039/b907335c

data_7002133
_publ_section_title
;
 Synthesis and structural studies of amido, hydrazido and imido
 zirconium(iv) complexes incorporating a diamido/diamine cyclam-based
 ligand
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              7494
_journal_page_last               7508
_journal_paper_doi               10.1039/b907335c
_journal_year                    2009
_chemical_formula_moiety         'C40 H53 Cl N6 Zr, C7 H8'
_chemical_formula_sum            'C47 H61 Cl N6 Zr'
_chemical_formula_weight         836.69
_chemical_name_systematic
;
(Bn2Cyclam)ZrCl(NPhNPhBu)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 101.019(18)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.978(6)
_cell_length_b                   15.349(8)
_cell_length_c                   26.502(15)
_cell_measurement_reflns_used    2379
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.16
_cell_measurement_theta_min      2.31
_cell_volume                     4383(4)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    ORTEP3
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.1146
_diffrn_reflns_av_sigmaI/netI    0.0975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            37951
_diffrn_reflns_theta_full        25.59
_diffrn_reflns_theta_max         25.59
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.351
_exptl_absorpt_correction_T_max  0.9658
_exptl_absorpt_correction_T_min  0.9331
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1768
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.385
_refine_diff_density_min         -0.412
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         8176
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0956
_refine_ls_R_factor_gt           0.0505
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.1089
_reflns_number_gt                5365
_reflns_number_total             8176
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b907335c.txt
_cod_data_source_block           Compound9
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7002133