Facilitated carbon dioxide reduction using a Zn(ii) complex.
Donovan, Elizabeth S.; Barry, Brian M.; Larsen, Christopher A.; Wirtz, Melissa N.; Geiger, William E.; Kemp, Richard A.; Chemical communications (Cambridge, England) 52 (2016) 1685–1688; doi:10.1039/c5cc07318a

data_7118519
_publ_section_title
;
 Facilitated carbon dioxide reduction using a Zn(ii) complex.
;
_journal_issue                   8
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1685
_journal_page_last               1688
_journal_paper_doi               10.1039/c5cc07318a
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         '2(C16 H13 Cl2 N2 P Zn), C4 H8 O'
_chemical_formula_sum            'C36 H34 Cl4 N4 O P2 Zn2'
_chemical_formula_weight         873.15
_chemical_melting_point          543.0(10)
_chemical_name_systematic
'dichloro[phenyldi(2-pyridyl)phosphine-2-N,N]zinc(II) '
_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
_audit_creation_date             2014-10-16
_audit_creation_method
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_audit_update_record
;
2014-10-17 deposited with the CCDC.
2015-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.966(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.0669(5)
_cell_length_b                   12.2540(4)
_cell_length_c                   19.5763(7)
_cell_measurement_reflns_used    6463
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.12
_cell_measurement_theta_min      2.29
_cell_volume                     3807.2(2)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0820
_diffrn_reflns_av_unetI/netI     0.0747
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            58715
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.604
_diffrn_reflns_theta_min         1.967
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.660
_exptl_absorpt_correction_T_max  0.8119
_exptl_absorpt_correction_T_min  0.4150
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker, SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1776
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/pentane'
_exptl_crystal_size_max          0.498
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.131
_refine_diff_density_max         1.057
_refine_diff_density_min         -0.975
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         11623
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.1165
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+13.9109P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1515
_refine_ls_wR_factor_ref         0.1727
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7059
_reflns_number_total             11623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc07318a2.cif
_cod_data_source_block           Compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '542-544' was changed to '543.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_database_code               7118519
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.812
_shelx_estimated_absorpt_t_min   0.492
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(O1) = Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36) = Uanis(O1A) =
Uanis(C34A) = Uanis(C35A)
3. Others
 Sof(H33C)=Sof(H33D)=Sof(O1A)=Sof(C34A)=Sof(H34C)=Sof(H34D)=Sof(C35A)=
 Sof(H35C)=Sof(H35D)=Sof(H36C)=Sof(H36D)=1-FVAR(1)
 Sof(H33A)=Sof(H33B)=Sof(O1)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(C35)=Sof(H35A)=
 Sof(H35B)=Sof(H36A)=Sof(H36B)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C33(H33C,H33D), C34(H34A,H34B), C35(H35A,H35B), C34A(H34C,
 H34D), C35A(H35C,H35D), C36(H36A,H36B), C36(H36C,H36D)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C10(H10),
 C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29),
 C30(H30), C31(H31)
;
_olex2_submission_special_instructions 'No special instructions were received'