Square planar Cu(i) stabilized by a pyridinediimine ligand.
Cheung, Pui Man; Berger, Robert F.; Zakharov, Lev N.; Gilbertson, John D.; Chemical communications (Cambridge, England) 52 (2016) 4156–4159; doi:10.1039/c6cc00271d

data_7118724
_publ_section_title
;
 Square planar Cu(i) stabilized by a pyridinediimine ligand.
;
_journal_issue                   22
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              4156
_journal_page_last               4159
_journal_paper_doi               10.1039/c6cc00271d
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C35 H46 Cu N4, F6 P, C4 H8 O'
_chemical_formula_sum            'C39 H54 Cu F6 N4 O P'
_chemical_formula_weight         803.37
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-12-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-01-11 deposited with the CCDC.
2016-02-08 downloaded from the CCDC.
;
_cell_angle_alpha                96.920(3)
_cell_angle_beta                 105.670(3)
_cell_angle_gamma                107.141(3)
_cell_formula_units_Z            2
_cell_length_a                   12.4078(19)
_cell_length_b                   13.287(2)
_cell_length_c                   14.052(2)
_cell_measurement_reflns_used    8045
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      19.14
_cell_measurement_theta_min      2.37
_cell_volume                     2080.5(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 1.000
_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  0.0725
_diffrn_reflns_av_unetI/netI     0.0923
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            48577
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.542
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark-red
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       cut-block
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details
;
 Flack x determined using 3695 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.057(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         14571
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0525
_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^)+(0.0563P)^2^+0.3530P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1096
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.987
_reflns_Friedel_fraction_full    0.962
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                9718
_reflns_number_total             14571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc00271d2.cif
_cod_data_source_block           mo_gilb226_0m
_cod_depositor_comments
'Adding full bibliography for 7118721--7118725.cif.'
_cod_original_cell_volume        2080.5(6)
_cod_database_code               7118724
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.929
_shelx_estimated_absorpt_t_min   0.830
_olex2_refinement_description
;
1. Shared sites
{C5S, C5A}
{C8S, C8A}
2. Others
 Fixed Sof: O2S(0.5) C5S(0.5) H5SA(0.5) H5SB(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5)
 C7S(0.5) H7SA(0.5) H7SB(0.5) C8S(0.5) H8SA(0.5) H8SB(0.5) O2A(0.5) C5A(0.5)
 H5AA(0.5) H5AB(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) C7A(0.5) H7AA(0.5) H7AB(0.5)
 C8A(0.5) H8AA(0.5) H8AB(0.5)
 Fixed Uiso: H1A(0.115) H1B(0.115) H1C(0.115) H4A(0.061) H5A(0.064) H6A(0.057)
 H9A(0.072) H9B(0.072) H9C(0.072) H12A(0.069) H13A(0.076) H14A(0.07)
 H16A(0.088) H17A(0.194) H17B(0.194) H17C(0.194) H18A(0.164) H18B(0.164)
 H18C(0.164) H19A(0.079) H20A(0.21) H20B(0.21) H20C(0.21) H21Q(0.165)
 H21R(0.165) H21S(0.165) H24A(0.075) H25B(0.076) H26A(0.076) H28A(0.086)
 H29A(0.168) H29B(0.168) H29C(0.168) H30A(0.123) H30B(0.123) H30C(0.123)
 H31A(0.071) H32A(0.164) H32B(0.164) H32C(0.164) H33A(0.15) H33B(0.15)
 H33C(0.15) H35A(0.088) H35B(0.088) H35C(0.088) H1'A(0.119) H1'B(0.119)
 H1'C(0.119) H4'A(0.074) H5'A(0.084) H6'A(0.068) H9'A(0.083) H9'B(0.083)
 H9'C(0.083) H12B(0.058) H13B(0.063) H14B(0.069) H16B(0.063) H17D(0.111)
 H17E(0.111) H17F(0.111) H18D(0.135) H18E(0.135) H18F(0.135) H19B(0.061)
 H20D(0.115) H20E(0.115) H20F(0.115) H21A(0.13) H21B(0.13) H21C(0.13)
 H24B(0.07) H25A(0.075) H26B(0.063) H28B(0.067) H29D(0.114) H29E(0.114)
 H29F(0.114) H30D(0.122) H30E(0.122) H30F(0.122) H31B(0.068) H32D(0.119)
 H32E(0.119) H32F(0.119) H33D(0.134) H33E(0.134) H33F(0.134) H35D(0.092)
 H35E(0.092) H35F(0.092) H1SA(0.118) H1SB(0.118) H2SA(0.183) H2SB(0.183)
 H3SA(0.189) H3SB(0.189) H4SA(0.221) H4SB(0.221) H5SA(0.178) H5SB(0.178)
 H6SA(0.092) H6SB(0.092) H7SA(0.177) H7SB(0.177) H8SA(0.198) H8SB(0.198)
 H5AA(0.178) H5AB(0.178) H6AA(0.15) H6AB(0.15) H7AA(0.189) H7AB(0.189)
 H8AA(0.198) H8AB(0.198)
 Fixed X: H1A(0.4427) H1B(0.4418) H1C(0.3607) H4A(0.2903) H5A(0.1507) H6A(-
 0.0125) H9A(-0.2313) H9B(-0.2095) H9C(-0.146) H12A(0.5751) H13A(0.5388)
 H14A(0.3822) H16A(0.3972) H17A(0.4827) H17B(0.5308) H17C(0.3905) H18A(0.589)
 H18B(0.5684) H18C(0.6465) H19A(0.1909) H20A(0.1002) H20B(0.1575) H20C(0.0602)
 H21Q(0.1996) H21R(0.3033) H21S(0.3273) H24A(-0.2304) H25B(-0.3766) H26A(-
 0.3851) H28A(-0.0205) H29A(0.0038) H29B(-0.0853) H29C(-0.1337) H30A(0.0913)
 H30B(0.0626) H30C(0.1423) H31A(-0.1916) H32A(-0.3583) H32B(-0.38) H32C(-
 0.4249) H33A(-0.2026) H33B(-0.2361) H33C(-0.1098) H35A(0.1779) H35B(0.3018)
 H35C(0.2024) H1'A(-0.2324) H1'B(-0.1341) H1'C(-0.167) H4'A(0.0368)
 H5'A(0.2347) H6'A(0.3745) H9'A(0.5122) H9'B(0.4698) H9'C(0.5043) H12B(-0.3039)
 H13B(-0.4468) H14B(-0.4261) H16B(-0.0349) H17D(0.0015) H17E(-0.1229) H17F(-
 0.0177) H18D(-0.1825) H18E(-0.2182) H18F(-0.0897) H19B(-0.2086) H20D(-0.1005)
 H20E(-0.2179) H20F(-0.1584) H21A(-0.3529) H21B(-0.4149) H21C(-0.4177)
 H24B(0.55) H25A(0.5347) H26B(0.4137) H28B(0.4375) H29D(0.5508) H29E(0.559)
 H29F(0.6231) H30D(0.3356) H30E(0.259) H30F(0.3292) H31B(0.2728) H32D(0.3882)
 H32E(0.2994) H32F(0.2525) H33D(0.1192) H33E(0.0889) H33F(0.1363) H35D(-0.0811)
 H35E(-0.1547) H35F(-0.1835) H1SA(0.7475) H1SB(0.8591) H2SA(0.8724)
 H2SB(0.9858) H3SA(1.0155) H3SB(0.9071) H4SA(0.7796) H4SB(0.8961) H5SA(0.3381)
 H5SB(0.4706) H6SA(0.4206) H6SB(0.3459) H7SA(0.1701) H7SB(0.2325) H8SA(0.2728)
 H8SB(0.1791) H5AA(0.458) H5AB(0.3999) H6AA(0.4302) H6AB(0.3207) H7AA(0.1942)
 H7AB(0.3027) H8AA(0.1735) H8AB(0.3121)
 Fixed Y: H1A(0.4901) H1B(0.3703) H1C(0.3921) H4A(0.1998) H5A(0.0299)
 H6A(0.0108) H9A(0.0759) H9B(0.049) H9C(0.0083) H12A(0.7427) H13A(0.8668)
 H14A(0.8129) H16A(0.4577) H17A(0.4981) H17B(0.6237) H17C(0.5597) H18A(0.4495)
 H18B(0.4748) H18C(0.5697) H19A(0.5366) H20A(0.6365) H20B(0.7388) H20C(0.6317)
 H21Q(0.63) H21R(0.7328) H21S(0.622) H24A(0.2431) H25B(0.3009) H26A(0.3329)
 H28A(0.1649) H29A(0.1382) H29B(0.2012) H29C(0.0882) H30A(0.3522) H30B(0.3632)
 H30C(0.2927) H31A(0.2831) H32A(0.276) H32B(0.18) H32C(0.2786) H33A(0.4396)
 H33B(0.4738) H33C(0.4595) H35A(0.7627) H35B(0.7633) H35C(0.7804) H1'A(0.7247)
 H1'B(0.7413) H1'C(0.8422) H4'A(0.9029) H5'A(1.0078) H6'A(1.0384) H9'A(1.04)
 H9'B(1.11) H9'C(1.009) H12B(0.4154) H13B(0.4663) H14B(0.6494) H16B(0.5975)
 H17D(0.4354) H17E(0.3929) H17F(0.4967) H18D(0.5237) H18E(0.4088) H18F(0.4604)
 H19B(0.8667) H20D(0.8607) H20E(0.8417) H20F(0.9533) H21A(0.9297) H21B(0.8148)
 H21C(0.8256) H24B(0.8432) H25A(0.9648) H26B(1.0675) H28B(0.8163) H29D(0.7027)
 H29E(0.7265) H29F(0.8213) H30D(0.6313) H30E(0.7016) H30F(0.6528) H31B(1.0887)
 H32D(1.2253) H32E(1.1687) H32F(1.2201) H33D(0.936) H33E(1.0441) H33F(0.9928)
 H35D(0.5519) H35E(0.5018) H35F(0.5949) H1SA(0.002) H1SB(-0.0149) H2SA(0.0768)
 H2SB(0.0857) H3SA(0.2549) H3SB(0.2479) H4SA(0.2252) H4SB(0.2785) H5SA(0.4135)
 H5SB(0.4339) H6SA(0.4672) H6SB(0.524) H7SA(0.3811) H7SB(0.3735) H8SA(0.2355)
 H8SB(0.2242) H5AA(0.4107) H5AB(0.4675) H6AA(0.286) H6AB(0.3139) H7AA(0.1896)
 H7AB(0.1596) H8AA(0.2394) H8AB(0.2634)
 Fixed Z: H1A(1.112) H1B(1.0789) H1C(1.1447) H4A(1.0428) H5A(0.9616)
 H6A(0.8219) H9A(0.633) H9B(0.7432) H9C(0.6689) H12A(0.9347) H13A(1.0408)
 H14A(1.1047) H16A(0.8515) H17A(0.727) H17B(0.7791) H17C(0.7318) H18A(0.8727)
 H18B(0.9793) H18C(0.9404) H19A(1.0689) H20A(0.9667) H20B(1.0597) H20C(1.0657)
 H21Q(1.229) H21R(1.224) H21S(1.2344) H24A(0.3734) H25B(0.407) H26A(0.5695)
 H28A(0.548) H29A(0.3866) H29B(0.3468) H29C(0.3772) H30A(0.6021) H30B(0.4865)
 H30C(0.5281) H31A(0.7838) H32A(0.8267) H32B(0.7354) H32C(0.7128) H33A(0.8657)
 H33B(0.7591) H33C(0.804) H35A(0.7242) H35B(0.7974) H35C(0.8438) H1'A(0.1204)
 H1'B(0.0642) H1'C(0.1056) H4'A(0.0906) H5'A(0.1213) H6'A(0.2799) H9'A(0.5421)
 H9'B(0.4643) H9'C(0.4262) H12B(0.2606) H13B(0.3136) H14B(0.3484) H16B(0.2409)
 H17D(0.2728) H17E(0.2937) H17F(0.3686) H18D(0.0825) H18E(0.1126) H18F(0.1011)
 H19B(0.3063) H20D(0.4708) H20E(0.5031) H20F(0.4748) H21A(0.3504) H21B(0.372)
 H21C(0.2593) H24B(0.7561) H25A(0.8801) H26B(0.8386) H28B(0.4913) H29D(0.5265)
 H29E(0.6431) H29F(0.5957) H30D(0.4712) H30E(0.4988) H30F(0.5837) H31B(0.5893)
 H32D(0.7389) H32E(0.796) H32F(0.7028) H33D(0.5976) H33E(0.6171) H33F(0.7104)
 H35D(0.6205) H35E(0.5031) H35F(0.564) H1SA(-0.0046) H1SB(-0.0336) H2SA(0.1489)
 H2SB(0.1118) H3SA(0.1105) H3SB(0.1549) H4SA(0.005) H4SB(-0.0252) H5SA(0.4985)
 H5SB(0.4933) H6SA(0.332) H6SB(0.3838) H7SA(0.3061) H7SB(0.2196) H8SA(0.2571)
 H8SB(0.317) H5AA(0.435) H5AB(0.5045) H6AA(0.5292) H6AB(0.5531) H7AA(0.4205)
 H7AB(0.3984) H8AA(0.2668) H8AB(0.2782)
;
_shelx_res_checksum              648
_olex2_submission_special_instructions 'No special instructions were received'