Syntheses and characterization of hepta-coordinated Group 4 amidinate complexes.
Cook, Tabitha M.; Steren, Carlos A.; Xue, Zi-Ling; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11030–11040; doi:10.1039/c8dt02523a

data_7047034
_publ_section_title
;
 Syntheses and characterization of hepta-coordinated Group 4 amidinate
 complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11030
_journal_page_last               11040
_journal_paper_doi               10.1039/c8dt02523a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C26 H56 N6 Zr'
_chemical_formula_sum            'C26 H56 N6 Zr'
_chemical_formula_weight         543.98
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     iterative
_audit_creation_date             2018-06-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-09 deposited with the CCDC.
2018-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.401(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.699(7)
_cell_length_b                   15.619(5)
_cell_length_c                   18.597(6)
_cell_measurement_reflns_used    9344
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.72
_cell_measurement_theta_min      2.33
_cell_volume                     6131(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 (Bruker, 2008)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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  0.0330
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            69813
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.740
_diffrn_reflns_theta_min         1.622
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.381
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1424 before and 0.0488 after correction. The Ratio of minimum to maximum transmission is 0.9197. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_description       block
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.552
_exptl_crystal_size_mid          0.382
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         14282
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0280P)^2^+3.3654P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0679
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12596
_reflns_number_total             14282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02523a2.cif
_cod_data_source_block           ZrAmid3Et
_cod_depositor_comments
'Adding full bibliography for 7047032--7047035.cif.'
_cod_database_code               7047034
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.817
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C45(H45), C22(H22), C6(H6), C40(H40), C29(H29), C32(H32), C48(H48), C14(H14),
 C3(H3), C37(H37), C19(H19), C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C51(H51A,H51B), C25(H25A,H25B)
2.c Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C24(H24A,H24B,H24C), C36(H36A,H36B,
 H36C), C52(H52A,H52B,H52C), C21(H21A,H21B,H21C), C46(H46A,H46B,H46C), C31(H31A,
 H31B,H31C), C49(H49A,H49B,H49C), C5(H5A,H5B,H5C), C26(H26A,H26B,H26C),
 C44(H44A,H44B,H44C), C47(H47A,H47B,H47C), C34(H34A,H34B,H34C), C42(H42A,H42B,
 H42C), C4(H4A,H4B,H4C), C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C),
 C33(H33A,H33B,H33C), C39(H39A,H39B,H39C), C10(H10A,H10B,H10C), C15(H15A,H15B,
 H15C), C7(H7A,H7B,H7C), C23(H23A,H23B,H23C), C13(H13A,H13B,H13C), C20(H20A,
 H20B,H20C), C41(H41A,H41B,H41C), C50(H50A,H50B,H50C), C16(H16A,H16B,H16C),
 C38(H38A,H38B,H38C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              36326
_olex2_submission_special_instructions 'No special instructions were received'