Asymmetric bis-PNP pincer complexes of zirconium and hafnium - a measure of hemilability.
Idelson, Celia; Webster, Leah; Krämer, Tobias; Chadwick, F. Mark; Dalton transactions (Cambridge, England : 2003) 49 (2020) 16653–16656; doi:10.1039/d0dt03544k

data_7705864
_publ_section_title
;
 Asymmetric bis-PNP pincer complexes of zirconium and hafnium - a measure
 of hemilability.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16653
_journal_page_last               16656
_journal_paper_doi               10.1039/d0dt03544k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C60 H52 Cl2 Hf1 N2 P4'
_chemical_formula_sum            'C60 H52 Cl2 Hf N2 P4'
_chemical_formula_weight         1174.38
_chemical_melting_point          ?
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_audit_creation_date             2020-03-06
_audit_creation_method           CRYSTALS_ver_14.61_build_6999
_audit_update_record
;
2020-08-18 deposited with the CCDC.	2020-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                84.873(4)
_cell_angle_beta                 86.804(5)
_cell_angle_gamma                66.482(5)
_cell_formula_units_Z            2
_cell_length_a                   11.07535(3)
_cell_length_b                   13.14605(3)
_cell_length_c                   20.39291(4)
_cell_measurement_reflns_used    3904
_cell_measurement_temperature    173
_cell_measurement_theta_max      71
_cell_measurement_theta_min      4
_cell_volume                     2710.97(10)
_computing_cell_refinement
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.940
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'focussing mirrors'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.069
_diffrn_reflns_av_unetI/netI     0.112
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15997
_diffrn_reflns_theta_full        25.072
_diffrn_reflns_theta_max         73.742
_diffrn_reflns_theta_min         3.677
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.885
_exptl_absorpt_correction_T_max  0.56
_exptl_absorpt_correction_T_min  0.36
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            yello
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         3.36
_refine_diff_density_min         -1.78
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.5867
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     677
_refine_ls_number_reflns         11601
_refine_ls_number_restraints     140
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.0102888
_refine_ls_shift/su_mean         0.0002721
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 914. 0.140E+04 852. 336. 55.5 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2571
_refine_ls_wR_factor_gt          0.2129
_refine_ls_wR_factor_ref         0.2571
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              -15
_reflns_limit_l_max              20
_reflns_limit_l_min              -25
_reflns_number_gt                8407
_reflns_number_total             11605
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.90
_oxford_diffrn_Wilson_scale      1.49
_oxford_refine_ls_r_factor_ref   0.1028
_oxford_refine_ls_scale          1.286(7)
_oxford_reflns_number_all        11601
_oxford_structure_analysis_title 'lve\FMC2003\FMC2003.cif_od At 10: 4 on 5/ 3'
_cod_data_source_file            d0dt03544k3.cif
_cod_data_source_block           PNP2HfCl2
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value 'not measured' was changed
to '?' -- the value is undefined or not given.

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        2710.96(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C60 H52 Cl2 Hf1 N2 P4'
_cod_database_code               7705864
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)