#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:31:35 +0100 (vie 25 de mar de 2016) $
#$Revision: 180083 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/29/7052987.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7052987
loop_
_publ_author_name
'Jacobs, Tia'
'Barbour, Leonard J.'
_publ_section_title
;
 Single-crystal to single-crystal transformations in discrete solvated
 metallocycles: the role of the metal ion
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              71
_journal_paper_doi               10.1039/c2nj40612h
_journal_volume                  37
_journal_year                    2013
_chemical_formula_moiety         'C44 H44 Cl4 N8 Zn2, 2(C H4 O)'
_chemical_formula_sum            'C46 H52 Cl4 N8 O2 Zn2'
_chemical_formula_weight         1021.50
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.97(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   17.36(2)
_cell_length_b                   15.483(20)
_cell_length_c                   9.440(12)
_cell_measurement_reflns_used    654
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.27
_cell_measurement_theta_min      2.36
_cell_volume                     2319(5)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics
;
X-Seed (Barbour, 2001; Atwood & Barbour, 2003)
;
_computing_publication_material
;
X-Seed (Atwood & Barbour, 2003; Barbour, 2001)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1075
_diffrn_reflns_av_sigmaI/netI    0.1528
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7139
_diffrn_reflns_theta_full        28.21
_diffrn_reflns_theta_max         28.21
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.313
_exptl_absorpt_correction_T_max  0.8479
_exptl_absorpt_correction_T_min  0.7021
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.463
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.803
_refine_diff_density_min         -1.071
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     150
_refine_ls_number_reflns         2778
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1368
_refine_ls_R_factor_gt           0.0859
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0748P)²+3.3583P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1777
_refine_ls_wR_factor_ref         0.1991
_reflns_number_gt                1809
_reflns_number_total             2778
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2nj40612h.txt
_cod_data_source_block           ZnCl2_MeOH
_cod_original_cell_volume        2318(5)
_cod_original_sg_symbol_H-M      C2/m
_cod_database_code               7052987
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cl2 Cl 0.12851(14) 0.0000 0.4888(3) 0.0316(5) Uani 1 2 d S
Cl3 Cl 0.33950(17) 0.0000 0.8465(3) 0.0393(6) Uani 1 2 d S
Zn1 Zn 0.27122(6) 0.0000 0.58223(11) 0.0205(3) Uani 1 2 d S
N4 N 0.3133(3) 0.1076(3) 0.5207(5) 0.0211(10) Uani 1 1 d .
C5 C 0.3849(4) 0.1530(4) 0.6173(7) 0.0305(15) Uani 1 1 d .
H5 H 0.4229 0.1353 0.7178 0.037 Uiso 1 1 calc R
C6 C 0.3916(4) 0.2257(4) 0.5455(8) 0.0310(15) Uani 1 1 d .
H6 H 0.4343 0.2685 0.5860 0.037 Uiso 1 1 calc R
N7 N 0.3246(3) 0.2265(3) 0.4012(6) 0.0221(11) Uani 1 1 d .
C8 C 0.2790(3) 0.1547(4) 0.3893(7) 0.0211(12) Uani 1 1 d .
C9 C 0.2023(4) 0.1303(4) 0.2510(7) 0.0300(15) Uani 1 1 d .
H9A H 0.1606 0.1769 0.2263 0.045 Uiso 1 1 calc R
H9B H 0.1784 0.0772 0.2728 0.045 Uiso 1 1 calc R
H9C H 0.2172 0.1208 0.1626 0.045 Uiso 1 1 calc R
C10 C 0.3088(4) 0.2957(4) 0.2867(7) 0.0247(14) Uani 1 1 d .
H10A H 0.3154 0.3521 0.3395 0.030 Uiso 1 1 calc R
H10B H 0.2498 0.2914 0.2091 0.030 Uiso 1 1 calc R
C11 C 0.3675(4) 0.2926(4) 0.2035(7) 0.0232(13) Uani 1 1 d .
C12 C 0.4142(4) 0.3646(3) 0.2027(7) 0.0211(13) Uani 1 1 d .
H12 H 0.4111 0.4152 0.2573 0.025 Uiso 1 1 calc R
C13 C 0.4657(3) 0.3631(3) 0.1218(7) 0.0226(13) Uani 1 1 d .
H13 H 0.4969 0.4133 0.1202 0.027 Uiso 1 1 calc R
C14 C 0.4723(3) 0.2899(3) 0.0438(7) 0.0190(12) Uani 1 1 d .
C15 C 0.4273(4) 0.2168(3) 0.0511(6) 0.0197(12) Uani 1 1 d .
H15 H 0.4334 0.1652 0.0022 0.024 Uiso 1 1 calc R
C16 C 0.3745(4) 0.2169(4) 0.1264(7) 0.0232(13) Uani 1 1 d .
H16 H 0.3431 0.1667 0.1267 0.028 Uiso 1 1 calc R
C17 C 0.4208(6) 0.0000 0.2945(13) 0.045(3) Uani 1 2 d S
H17A H 0.4353 0.0575 0.3414 0.068 Uiso 0.50 1 calc PR
H17B H 0.4585 -0.0148 0.2439 0.068 Uiso 0.50 1 calc PR
H17C H 0.4272 -0.0427 0.3752 0.068 Uiso 0.50 1 calc PR
O18 O 0.3334(4) 0.0000 0.1792(9) 0.0495(19) Uani 1 2 d S
H18 H 0.3316 -0.0181 0.0941 0.059 Uiso 0.50 1 calc PR
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N4 Zn1 N4 113.0(3) . 6
N4 Zn1 Cl2 110.97(14) . .
N4 Zn1 Cl2 110.97(14) 6 .
N4 Zn1 Cl3 103.20(15) . .
N4 Zn1 Cl3 103.20(15) 6 .
Cl2 Zn1 Cl3 115.14(10) . .
C8 N4 C5 105.8(5) . .
C8 N4 Zn1 129.8(4) . .
C5 N4 Zn1 124.3(4) . .
C6 C5 N4 109.2(6) . .
C6 C5 H5 125.4 . .
N4 C5 H5 125.4 . .
C5 C6 N7 107.0(5) . .
C5 C6 H6 126.5 . .
N7 C6 H6 126.5 . .
C8 N7 C6 107.8(5) . .
C8 N7 C10 128.0(5) . .
C6 N7 C10 124.2(5) . .
N7 C8 N4 110.2(5) . .
N7 C8 C9 124.8(5) . .
N4 C8 C9 125.0(5) . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
N7 C10 C11 113.3(5) . .
N7 C10 H10A 108.9 . .
C11 C10 H10A 108.9 . .
N7 C10 H10B 108.9 . .
C11 C10 H10B 108.9 . .
H10A C10 H10B 107.7 . .
C12 C11 C16 119.6(5) . .
C12 C11 C10 119.7(5) . .
C16 C11 C10 120.6(5) . .
C11 C12 C13 119.9(5) . .
C11 C12 H12 120.1 . .
C13 C12 H12 120.1 . .
C14 C13 C12 121.2(5) . .
C14 C13 H13 119.4 . .
C12 C13 H13 119.4 . .
C13 C14 C15 118.1(5) . .
C13 C14 C14 120.3(4) . 2_655
C15 C14 C14 121.6(4) . 2_655
C16 C15 C14 122.1(5) . .
C16 C15 H15 118.9 . .
C14 C15 H15 118.9 . .
C15 C16 C11 119.0(5) . .
C15 C16 H16 120.5 . .
C11 C16 H16 120.5 . .
O18 C17 H17A 109.5 . .
O18 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
O18 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C17 O18 H18 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cl2 Zn1 2.267(4) .
Cl3 Zn1 2.286(4) .
Zn1 N4 1.999(5) .
Zn1 N4 1.999(5) 6
N4 C8 1.351(7) .
N4 C5 1.396(8) .
C5 C6 1.343(9) .
C5 H5 0.9500 .
C6 N7 1.386(8) .
C6 H6 0.9500 .
N7 C8 1.343(7) .
N7 C10 1.466(7) .
C8 C9 1.486(8) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C9 H9C 0.9800 .
C10 C11 1.518(8) .
C10 H10A 0.9900 .
C10 H10B 0.9900 .
C11 C12 1.380(8) .
C11 C16 1.411(8) .
C12 C13 1.393(8) .
C12 H12 0.9500 .
C13 C14 1.381(8) .
C13 H13 0.9500 .
C14 C15 1.393(7) .
C14 C14 1.501(10) 2_655
C15 C16 1.369(8) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C17 O18 1.465(12) .
C17 H17A 0.9800 .
C17 H17B 0.9800 .
C17 H17C 0.9800 .
O18 H18 0.8400 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O18 H18 Cl3 0.84 2.41 3.186(9) 153.2 1_554
