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_7705863
_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         'C34 H34 Li1 N1 O1 P2'
_chemical_formula_sum            'C34 H34 Li N O P2'
_chemical_formula_weight         541.54
_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             2020-07-06
_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                94.396(4)
_cell_angle_beta                 105.416(4)
_cell_angle_gamma                114.647(4)
_cell_formula_units_Z            2
_cell_length_a                   10.70733(3)
_cell_length_b                   10.84431(3)
_cell_length_c                   14.74442(3)
_cell_measurement_reflns_used    3783
_cell_measurement_temperature    173
_cell_measurement_theta_max      73
_cell_measurement_theta_min      5
_cell_volume                     1465.32(7)
_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 0.935
_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  0.027
_diffrn_reflns_av_unetI/netI     0.050
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8327
_diffrn_reflns_theta_full        41.086
_diffrn_reflns_theta_max         73.368
_diffrn_reflns_theta_min         4.593
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.545
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 CrysAlisPro (Rigaku Oxford Diffraction, 2017) 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             572
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.50
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.4590
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         5524
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.0004157
_refine_ls_shift/su_mean         0.0000385
_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: 
 836. 0.130E+04 722. 245. 34.8 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1005
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.1005
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                4372
_reflns_number_total             5524
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.63
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0566
_oxford_refine_ls_scale          5.19(6)
_oxford_reflns_number_all        5524
_oxford_structure_analysis_title C:\Users\fchadwic\Desktop\solve\FMC2004.cif_
_cod_data_source_file            d0dt03544k3.cif
_cod_data_source_block           LiPNPPh
_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        1465.32(8)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C34 H34 Li1 N1 O1 P2'
_cod_database_code               7705863
_oxford_refine_reflns_threshold_expression_ref I>-3.0\s(I)