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_7705862
_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 N2 P4 Zr1'
_chemical_formula_sum            'C60 H52 Cl2 N2 P4 Zr'
_chemical_formula_weight         1087.11
_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_update_record
;
2020-08-18 deposited with the CCDC.	2020-11-10 downloaded from the CCDC.
;
_cell_angle_alpha                85.224(4)
_cell_angle_beta                 86.838(4)
_cell_angle_gamma                66.436(6)
_cell_formula_units_Z            2
_cell_length_a                   11.1053(7)
_cell_length_b                   13.1355(8)
_cell_length_c                   20.3905(10)
_cell_measurement_reflns_used    6386
_cell_measurement_temperature    173
_cell_measurement_theta_max      73
_cell_measurement_theta_min      4
_cell_volume                     2716.2(3)
_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 0.994
_diffrn_measured_fraction_theta_max 0.947
_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  0.039
_diffrn_reflns_av_unetI/netI     0.068
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            15595
_diffrn_reflns_theta_full        43.321
_diffrn_reflns_theta_max         73.426
_diffrn_reflns_theta_min         3.679
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.982
_exptl_absorpt_correction_T_max  0.67
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.78
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.6170
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     622
_refine_ls_number_reflns         10316
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.0010450
_refine_ls_shift/su_mean         0.0000239
_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: 
 650. 0.101E+04 578. 210. 33.1 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1274
_refine_ls_wR_factor_gt          0.1134
_refine_ls_wR_factor_ref         0.1274
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                8347
_reflns_number_total             10361
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.29
_oxford_diffrn_Wilson_scale      0.24
_oxford_refine_ls_r_factor_ref   0.0562
_oxford_refine_ls_scale          2.074(10)
_oxford_reflns_number_all        10316
_oxford_structure_analysis_title
'lve\FMC2002\FMC2002.cif_od At 11:37 on 20/ 1'
_cod_data_source_file            d0dt03544k3.cif
_cod_data_source_block           PNP2ZrCl2
_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_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C60 H52 Cl2 N2 P4 Zr1'
_cod_database_code               7705862
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)
_platon_squeeze_void_probe_radius 1.20