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_7002131
_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         '2(C36 H52 Cl N5 Zr), 3(C4 H10 O)'
_chemical_formula_sum            'C84 H134 Cl2 N10 O3 Zr2'
_chemical_formula_weight         1585.35
_chemical_name_systematic
;
(Bn2Cyclam)Zr(NH2,6iPrPh)Cl
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 104.543(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.7286(8)
_cell_length_b                   28.7142(17)
_cell_length_c                   20.8751(12)
_cell_measurement_reflns_used    6194
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.38
_cell_measurement_theta_min      2.14
_cell_volume                     8545.6(9)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0723
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            82745
_diffrn_reflns_theta_full        25.76
_diffrn_reflns_theta_max         25.76
_diffrn_reflns_theta_min         2.02
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  0.9651
_exptl_absorpt_correction_T_min  0.9003
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3384
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     929
_refine_ls_number_reflns         16261
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0892
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+19.6424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1494
_reflns_number_gt                11937
_reflns_number_total             16261
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b907335c.txt
_cod_data_source_block           Compound6
_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_cell_volume        8545.6(8)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7002131